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Chemical Structure| 69506-91-8
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Product Details of [ 69506-91-8 ]

CAS No. :69506-91-8 MDL No. :MFCD23103199
Formula : C12H10N4 Boiling Point : -
Linear Structure Formula :(C3H3N2)2C6H4 InChI Key :GDWGYEKGZJOUHE-UHFFFAOYSA-N
M.W : 210.23 Pubchem ID :11333294
Synonyms :

Safety of [ 69506-91-8 ]

Signal Word:Warning Class:N/A
Precautionary Statements:P261-P280-P301+P312-P302+P352-P305+P351+P338 UN#:N/A
Hazard Statements:H302-H315-H319-H335 Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 69506-91-8 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 69506-91-8 ]

[ 69506-91-8 ] Synthesis Path-Downstream   1~100

  • 1
  • [ 288-32-4 ]
  • [ 108-36-1 ]
  • [ 69506-91-8 ]
YieldReaction ConditionsOperation in experiment
88% With potassium carbonate; copper(II) oxide; In dimethyl sulfoxide; at 150℃; for 48h; To a solution of <strong>[108-36-1]1,3-dibromobenzene</strong> (25.0mL, 210mmol) in DMSO (200mL) were added 1H-imidazole (35.0g, 510mmol), potassium carbonate (72.0g, 520mmol) and Cu(II) oxide (2.00g, 25.2mmol). After 48 h at 150 C, the solvent was removed by distillation. The crude solid was dissolved in dichloromethane (inorganic salts were insoluble) and the solution was filtered through Celite and concentrated. The product was precipitated from pentane as pale yellow powder (38.3g, 0.18mol). Yield: 88%. 1H NMR (300MHz, CDCl3): delta 7.95 (s, 2H, NCHN), 7.63 (m, 1H, CHaryl), 7.51 (t, J=2.0Hz, 1H, CHaryl), 7.45 (d, J=2.1Hz, 1H, CHaryl), 7.42 (d, J=1.8Hz, 1H, CHaryl), 7.39 (t, J=1.3Hz, 2H, CHimidazole), 7.25 (s, 1H, CHimidazole). 13C{1H} NMR (75MHz, CDCl3): delta 138.5 (NCHN), 135.4 (Caryl), 131.3 (CHimidazole), 130.8 (CHimidazole), 119.8 (CHaryl), 117.9 (CHaryl), 114.2 (CHaryl).
77% With potassium carbonate; copper(II) oxide; In dimethyl sulfoxide; at 150℃; for 48h; Raw Material 211 (2.5 ml, 21 mmol), Raw Material 221 (3.5 g, 52 mmol), K2C03 (7.2 g, 52 mmol) and CuO (0.4 g, 5.2 mmol) were mixed and dissolved in DMSO (20 ml). The solution was heated at 150 C for 48 hours. The reaction was cooled, and the DMSO was distilled at low-pressure, yielding an off-white solid. Chromatography on silica gel (25 1)eluting with CH2CI2/MeOH (10 1) gave a white solid (3.3 g, 77%) 1H NMR (400 MHz, CDCI3): 6 =7.91 (s, 2H), 7.60 (t, J = 8.0 Hz, 2H), 7.36-7.47 (m, 3H), 7.32 (s, 2H), 7.23 (s, 2H)
71.36% With copper(l) iodide; potassium carbonate; In dimethyl sulfoxide; at 120℃; for 48h; General procedure: A solution of 1, 3-dibromobenzene (4.718 g, 20 mmol), imidazole (2.996 g, 44 mmol), K2CO3 (8.293 g, 60 mmol) and CuI (0.762 g, 4 mmol) in DMSO (50 mL) was stirred vigorously at 120 C for 48 h. The reaction mixture after cooling to room temperature was filtered to give a clear solution which was treated with CH2Cl2 (300 mL) and deionized water (300 mL) to give an organic-aqueous biphasic solution. The collected organic phase was stripped of the solvent under vacuum, and the obtained residue was purified by column chromatography on silica gel, using CH2Cl2/ethanol (30:1) as an eluent, to afford the product of 1,3-di-imidazolyl benzene as a white solid (3.0 g, yield of 71.3%).
69% With copper(l) iodide; dimethylaminoacetic acid; potassium carbonate; A Schlenk flask was loaded with CuI (2.74 g, 14.4 mmol), N,N-dimethylglycine (2.97 g, 28.8 mmol), K2CO3 (39.79 g, 288 mmol) and imidazole (12.24 g, 180 mmol). The system was evacuated and filled with argon. 1,3-Dibromobenzene (16.92 g, 72 mmol) and 350 mL DMSO were added. The mixture was heated at 393 K for 48 h. After that the mixture was cooled down to room temperature and segregated between water and ethyl acetate. The organic layer was separated and the aqueous fraction was extracted with ethyl acetate twice. The combined organic layers were washed with NaHCO3, dried over MgSO4 and concentrated in vacuum. The residue was purified by column chromatography (dichlormethane/methanol (10:1)) and recrystallized from methanol to give white crystals of 1,3-bib. Yield 69% (based on <strong>[108-36-1]1,3-dibromobenzene</strong>).

  • 2
  • [ 100-39-0 ]
  • [ 69506-91-8 ]
  • 1,3-bis(1-benzylimidazol-3-yl)benzene dibromide [ No CAS ]
  • 3
  • [ 4206-67-1 ]
  • [ 69506-91-8 ]
  • C20H32N4Si2(2+)*2I(1-) [ No CAS ]
  • 4
  • [ 69506-91-8 ]
  • [ 74-88-4 ]
  • 1,1’-(1,3-phenylene)bis(3-methyl-1H-imidazol-3-ium) iodide [ No CAS ]
YieldReaction ConditionsOperation in experiment
98% In tetrahydrofuran; at 100℃; for 48h;Sealed tube; A sealed tube was charged with 1 ,3-bis(imidazole)benzene (0.42 g, 2 mmol) andiodomethane (1.2 ml, 8 mmol). After addition of 5 ml THF the tube was sealed and the reaction mixture stirred for 48 h at 100 C. The generated solid was filtered off and washedwith small portions of tetrahydrofuran and diethyl ether. After drying under vacuum anoff-white solid was yielded (0.97 g, 98%). 1H-NMR (d6'"DMSO, 600.16 MHz): o = 9.90 (s,2H, NCHN), 8.38 (s, 2H, CH), 8.31 (s, 1 H, CHarom.), 8.03 (s, 2H, CH), 8.00 (m, 3H), 3.99 (s,6H, CH3) ppm. 13C-NMR (d6'"DMSO, 150.91 MHz): o = 136.4 (NCHN), 135.8 (Ci), 132.1(CHarom.), 124.8 (CH), 122.6 (CHarom.), 121.0 (CH), 115.7 (CHarom.), 36.3 (CH3) ppm. M.p.266-269 C. Anal. Calc. for C14H16I2N4 (494.12 g mol-1): C, 34.03; H, 3.26; N, 11.34. Found:C, 33.88; H, 3.19; N, 11.32 %.
85% In dimethyl sulfoxide; ethyl acetate; at 20℃; for 48h;Inert atmosphere; HL7: Methyl iodide (3 equiv) was syringed into a 50 mL round-bottomed flask charged with HL6 (10 mmol) and DMSO (30 mL). The reaction was stirred under nitrogen in room temperature for 48 h. The mixture was poured into EtOAc (60 mL), and the white precipitate was formed, filtered, washed with ether, and air-dried to obtain HL7 in 85% yield. 1H NMR (DMSO): 3.99 (s, 6H), 7.97-8.00 (m, 3H), 8.00 (s, 2H), 8.31 (s, 1H), 8.37 (s, 2H), 9.89 (s, 2H).
66% In tetrahydrofuran; at 70℃; for 12h; The intermediate compound [L2-1](1.0eq) andMethyl iodide (5.0eq)Dissolved in THF (1.0M),And then, it was stirred at a temperature of 70C for 12 hours.The reaction mixture was cooled to room temperature,And then the extraction process was performed three times using dichloromethane and water to obtain an organic layer.The obtained organic layer was dried and concentrated by using magnesium sulfate, and using column chromatography,To obtain the intermediate compound [L2] (yield: 66%).
  • 5
  • [ 288-32-4 ]
  • [ 626-00-6 ]
  • [ 69506-91-8 ]
  • 1-(3-iodophenyl)-1H-imidazole [ No CAS ]
  • 6
  • [ 542-69-8 ]
  • [ 69506-91-8 ]
  • 1,1'-(1,3-phenylene)bis(3-butyl-1H-imidazol-3-ium)iodide [ No CAS ]
YieldReaction ConditionsOperation in experiment
68% In tetrahydrofuran; for 48h;Reflux; General procedure: <strong>[69506-91-8]1,3-di(imidazol-1-yl)benzene</strong> (4.00g, 19.0mmol) and n-butyl chloride (10.2mL, 98.1mmol) were stirred, in refluxing chlorobenzene, for 72h. After evaporation under reduced pressure, the crude solid was dissolved in dichloromethane containing few drops of methanol. An off-white powder was obtained after precipitation from Et2O (4.89g, 12.3mmol). Yield: 65%.
  • 7
  • [ 69506-91-8 ]
  • [ 1027018-97-8 ]
  • 8
  • [ 69506-91-8 ]
  • 1,3-bis[2-(1-oxyl-4,4,5,5-tetramethylimidazolin-2-yl)imidazol-1-yl]benzene [ No CAS ]
  • 9
  • [ 69506-91-8 ]
  • [ 199541-50-9 ]
  • 10
  • [ 288-32-4 ]
  • [ 626-00-6 ]
  • [ 69506-91-8 ]
YieldReaction ConditionsOperation in experiment
70% With copper(l) iodide; dimethylaminoacetic acid; potassium carbonate; In dimethyl sulfoxide; at 130℃; for 48h;Inert atmosphere; A mixture of CuI (228mg, 1.2mmol), N,N-dimethylglycine (350mg, 2.4mmol), K2CO3 (4.2g, 30mmol), imidazole (1.24g, 18mmol), and 1,3-diiodobenzene (2g, 6mmol) in 50mL DMSO was heated at 130C for 48h under N2 atmosphere in a round bottom flask. Then the mixture was cooled down to room temperature and partitioned between water (50mL) and ethyl acetate (100mL). The organic layer was separated and the aqueous fraction was extracted with ethyl acetate twice (2 x 50mL). The combined organic layers were washed with NaHCO3, dried over Na2SO4 and concentrated in vacuum which leads to an off white powder of the ligand, L. Yield: (0.882g, 70%) (based on 1,3-diiodobenzene).
61.3% With copper(I) oxide; potassium hydroxide; In dimethyl sulfoxide; at 120℃; for 48h;Inert atmosphere; A dried schlenk tube was charged with 1 ,3-diiodobenzene (3.30 g, 10 mmol), imidazole (2.04 g, 30 mmol), potassium hydroxide (2.24 g, 40 mmol) and copper(l) oxide (0.29 g,2 mmol) under an argon atmosphere and dry DMSO was added through a septum after anadditional degassing phase of the solids. The suspension was stirred for 48 hours at120 C. After cooling to room temperature the reaction mixture was poured into awater/ethyl acetate solution (1 :3). Solids were filtered off and the phases separated. The aqueous phase was extracted with ethyl acetate (3x50 ml), organic phases were combined,washed with brine (50 ml) and dried over magnesium sulfate. The crude product waspurified by flash chromatography with ethyl acetate yielding a pale crystalline solid (1.29 g,61.3%). 1H-NMR (CDCb, 300.13 MHz): o = 7.93 (s, 2H, NCHN), 7.62 (t, J = 7.9 Hz, 1 H,CHarom.), 7.43 (s, 2H), 7.41 (s, 1 H, CHarom.), 7.33 (s, 2H), 7.24 (s, 2H) ppm. 13C-NMR (CDCb, 75.475 MHz): o = 138.7 (Ci), 135.5 (NCHN), 131.5 (CHarom.), 131.0 (CHarom.),120.2 (CHarom.), 118.1 (CHarom.), 114.6 (CHarom.) ppm. M.p. 129-131 C. Anal. Calc. forC12H10N4 (210.24 g mol-1): C, 68.56; H, 4.79; N, 26.65. Found: C, 68.35; H, 4.74;N, 26.75%.
  • 13
  • [ 109-65-9 ]
  • [ 69506-91-8 ]
  • 1,1'-(1,3-phenylene)bis(3-butyl-1H-imidazol-3-ium)bromide [ No CAS ]
YieldReaction ConditionsOperation in experiment
92% With air; In acetonitrile; for 3h;Reflux; Inert atmosphere; Schlenk technique; 1,3-Bis(imidazol-1′-yl) benzene (3.73g, 17.8mmol), 1-bromobutane (19.0mL, 178mmol) and acetonitrile (150mL) were combined in air and stirred at reflux for 3h. After cooling to room temperature, the volatiles were removed under reduced pressure yielding a white solid (7.91g, 92%): 1H NMR (CDCl3, 300MHz): δ 11.44 (s, 2H), 9.13 (s, 2H), 9.00 (s, 1H), 8.36 (d, J=7.8Hz, 2H), 7.64 (t, J=8.1Hz, 1H), 7.58 (s, 2H), 4.46 (s, 4H), 2.02 (s, 4H), 1.44 (sex, J=7.8Hz, 4H), 0.99 (t, J=7.6Hz, 6H); 13C{1H} (75.5MHz, CD2Cl2): δ 136.1, 135.9, 132.9, 122.9, 122.8, 122.6, 114.9, 50.6, 32.2, 19.7, 13.6.
88% In toluene; at 150℃; for 48h;Reflux; The suspension of Intermediate 231 (4.3 g, 20.5 mmol) and 1-bromobutane (8.4 g, 61.3 mmol) in toluene was refluxed at 150 C for 48 hours. The solid stuck to the bottom of the flask. Solvent was poured out and the solid was washed by THF in order to wash out the viscous elements. The result was to obtain a white solid. Yield: 9.5g. 18 mmol; 88%. 1H NMR (400 MHz, CD3CN): 6 =10.84 (s, 2H), 8.79 (s, 1H), 8.36 (d, 2H), 7.94 (d, J= 7.68 Hz, 2H), 7.84 (t, J = 7.20 Hz, 1H), 7.65 (s, 2H), 4.31 (t, J = 7.20 Hz, 2H), 1.99 (quint, J = 7.52 Hz, 4H), 1.40 (sext, J = 7.56 Hz, 4H), 0.98 (t, J = 7.28 Hz, 6H)
80% In acetonitrile; at 90℃; for 12h;Schlenk technique; Inert atmosphere; Add 1,3-bisimidazole-1-ylbenzene (5.8g, 27.6mmol) to a 25mL Schlenk tube with a magnet,bromo-n-butane (18.9 g, 138 mmol) and acetonitrile (15 mL). The solution was heated to 90C under a nitrogen atmosphere with continuous stirring.After 12 hours, the acetonitrile was removed by rotary evaporation, and the solid residue was dissolved in 50 mL of ethanol.Concentrate again to approximately 5 mL volume and add 20 mL ether. The white precipitate was quickly collected as the target product (yield: 10.7 g, yield: 80%).
80% In acetonitrile; at 90℃; for 12h;Schlenk technique; Inert atmosphere; 1,3-bisimidazol-1-ylbenzene 5.8g, 27.6mmol), n-bromobutane (18.9g, 138mmol) and acetonitrile (15mL) were added to the 25mL Schlenk tube with magneton ). The solution was heated to 90C under nitrogen with continuous stirring. After 12 hours, the acetonitrile was removed by rotary evaporation, the solid residue was dissolved in 50 mL of ethanol, concentrated to a volume of about 5 mL, and 20 mL of ether was added. The white precipitate was quickly collected as the target product (yield: 10.7 g, yield: 80%)
63% In tetrahydrofuran; for 72h;Reflux; General procedure: <strong>[69506-91-8]1,3-di(imidazol-1-yl)benzene</strong> (4.00g, 19.0mmol) and n-butyl chloride (10.2mL, 98.1mmol) were stirred, in refluxing chlorobenzene, for 72h. After evaporation under reduced pressure, the crude solid was dissolved in dichloromethane containing few drops of methanol. An off-white powder was obtained after precipitation from Et2O (4.89g, 12.3mmol). Yield: 65%.

  • 14
  • [ 109-69-3 ]
  • [ 69506-91-8 ]
  • 1,1'-(1,3-phenylene)bis(3-butyl-1H-imidazol-3-ium)chloride [ No CAS ]
YieldReaction ConditionsOperation in experiment
91% In acetonitrile; at 160℃; for 24h;Inert atmosphere; Schlenk technique; Sealed tube; 1,3-Bis(imidazol-1′-yl) benzene (3.94g, 18.7mmol), 1-chlorobutane (39.0mL, 375mmol) and acetonitrile (250mL) were combined and stirred for 24h at 160C in a sealed tube. After cooling to room temperature, the volatiles were removed under reduced pressure yielding a white solid (6.71g, 91%): Spectroscopic data of imidazolium salt 2c were identical to previously published data [14d].
65% In chlorobenzene; at 130℃; for 72h; <strong>[69506-91-8]1,3-di(imidazol-1-yl)benzene</strong> (4.00g, 19.0mmol) and n-butyl chloride (10.2mL, 98.1mmol) were stirred, in refluxing chlorobenzene, for 72h. After evaporation under reduced pressure, the crude solid was dissolved in dichloromethane containing few drops of methanol. An off-white powder was obtained after precipitation from Et2O (4.89g, 12.3mmol). Yield: 65%. 1H NMR (500MHz, CD2Cl2): δ 11.76 (s, 2H, NCHN), 9.27 (s, 2H, CHimidazole), 9.11 (t, J=2.0Hz, 1H, CHaryl), 8.27 (dd, J=8.2Hz, 1.9Hz, 2H, CHaryl), 7.80 (s, 2H, CHimidazole), 7.54 (t, J=8.3Hz, 1H, CHaryl), 4.43 (t, J=7.3Hz, 4H, NCH2Bu), 2.04-1.92 (m, 4H, CH2Bu), 1.44-1.32 (m, 4H, CH2Bu), 0.93 (t, J=7.4Hz, 6H, CH3Bu). 13C{1H} NMR (126MHz, CD2Cl2): δ 137.0 (Caryl), 136.4 (NCHN), 132.5 (CHaryl), 123.5 (CHimidazole), 122.3 (CHaryl), 122.0 (CHimidazole), 114.7 (CHaryl), 50.6 (NCH2Bu), 32.3 (CH2Bu), 19.9 (CH2Bu), 13.7 (CH3Bu).
  • 18
  • [ 1079-66-9 ]
  • [ 69506-91-8 ]
  • [ 1415966-23-2 ]
YieldReaction ConditionsOperation in experiment
44% Under nitrogen atmosphere, to the solution of 1,3-di-imidazolylbenzene (2.0126 g, 10 mmol) in dry THF (150 mL) cooled to -78Cwas added dropwise with N, N, N, N-tetramethylethylenediamine(TMEDA, 3.0 mL, 20 mmol) and n-BuLi (2.5 M in hexane, 8.8 mL,22 mmol). The obtained mixture after stirring vigorously for 1 h,chlorodiphenylphosphine (PPh2Cl, 4.953 g, 22 mmol) was addeddropwise. The resultant mixture was stirred overnight with thereaction temperature increasing to ambient. After quenchingexcess n-BuLi with deionized water, the obtained oily mixture wasremoved of solvent in vacuo. The residue was purified by columnchromatography on silica gel, using CH2Cl2/ethyl acetate (30:1)as an eluent, to yield L1 as a white solid (2.53 g, 44%).1H NMR(400 MHz, , ppm, CD3CN): = 7.47 (t, J = 8 Hz, 1H, HPh), 7.32-7.36(m, 24H, HPh + imi), 7.26 (s, 2H, Himi), 7.18 (s, 1H, HPh).31P NMR(162 MHz, , ppm, CDCl3): = -28.2 (s, PPh2). The31P NMR signalof L1 ( = -28.2 ppm) observed herein was consistent to the onereported by Chauvin [24] with two phosphine fragments located intrans-position but different to the one reported by us [30] with twophosphine fragments located in cis-position.
  • 19
  • cobalt(II) chloride hexahydrate [ No CAS ]
  • [ 69506-91-8 ]
  • Co(1,3-bis(imidazol-1-yl)benzene)Cl2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
55% In N,N-dimethyl-formamide; at 79.84℃; for 48h; CoCl2·6H2O (23.7mg, 0.1mmol) and 1,3-<strong>[69506-91-8]bib</strong> (21mg 0.1mmol) were dissolved separately in DMF (2mL). The mixture was sonicated for 1min and heated at 353K for 48h. After cooling to room temperature the product was isolated by decanting the mother liquor and washed with DMF. For elemental analysis and TGA the product was dried under argon at room temperature for 6h. Yield 55% (based on 1,3-<strong>[69506-91-8]bib</strong>). Elemental analysis Calc. (%) for C12H10N4Cl2Co (Co(1,3-<strong>[69506-91-8]bib</strong>)Cl2): C 42.38; H 2.96; N 16.47. Found: C 42.53; H 2.86; N 16.45.
  • 20
  • cobalt(II) nitrate hexahydrate [ No CAS ]
  • [ 69506-91-8 ]
  • [ 33513-42-7 ]
  • Co(1,3-bis(imidazol-1-yl)benzene)(NO3)2(DMF)2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
86% In N,N-dimethyl-formamide; at 99.84℃; for 24h; Co(NO3)2·6H2O (26.2mg, 0.1mmol) and 1,3-<strong>[69506-91-8]bib</strong> (21mg, 0.1mmol) were dissolved separately in DMF (2mL). The mixture was sonicated for 1min and heated at 373K for 24h. After cooling to room temperature the product was isolated by decanting the mother liquor and washed with DMF. For elemental analysis and TGA the product was dried under argon at room temperature for 6h. Yield 86% (based on 1,3-<strong>[69506-91-8]bib</strong>). Elemental analysis Calc. (%) for C30H34O8N12Co (Co(1,3-<strong>[69506-91-8]bib</strong>)(NO3)2(DMF)2): C 48.09; H 4.57; N 22.43. Found: C 48.16; H 4.40; N 22.30
  • 21
  • cobalt(II) nitrate hexahydrate [ No CAS ]
  • [ 100-21-0 ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • [ 33513-42-7 ]
  • [Co(1,3-bis(imidazol-1-yl)benzene)(1,4-benzenedicarboxylate)](DMF)0.5(H2O)0.5 [ No CAS ]
YieldReaction ConditionsOperation in experiment
81% In N,N-dimethyl-formamide; at 119.84℃; for 48h;Autoclave; Co(NO3)2·6H2O (26.2mg, 0.1mmol) and H2(1,4-bdc) (16.6mg, 0.1mmol) were dissolved in 9mL DMF. 1,3-<strong>[69506-91-8]bib</strong> (21mg, 0.1mmol) was dissolved separately in 1mL DMF. After sonification for 1min the solutions were mixed, transferred into a Teflon vessel (25cm3) and heated in an autoclave at 393K for 48h. After cooling to room temperature the product was isolated by decanting the mother liquor and washed with DMF. For elemental analysis and TGA the product was dried under argon at room temperature for 6h. Yield 81% (based on 1,3-<strong>[69506-91-8]bib</strong>). Elemental analysis Calc. (%) for C20H14O4N4Co (Co(1,3-<strong>[69506-91-8]bib</strong>)(1,4-bdc)(DMF)0.5(H2O)0.5): C 53.93; H 3.89; N 13.16. Found: C 54.05; H 3.61; N 13.08.
  • 22
  • cobalt(II) nitrate hexahydrate [ No CAS ]
  • [ 1141-38-4 ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • [ 33513-42-7 ]
  • [Co(1,3-bis(imidazol-1-yl)benzene)(2,6-naphthalenedicarboxylate)](DMF)1.5(H2O)1.5 [ No CAS ]
YieldReaction ConditionsOperation in experiment
81% In N,N-dimethyl-formamide; at 119.84℃; for 48h;Autoclave; Co(NO3)2·6H2O (26.2mg, 0.1mmol) and H2(2,6-ndc) (21.6mg, 0.1mmol) were dissolved in 9mL DMF. 1,3-<strong>[69506-91-8]bib</strong> (21mg, 0.1mmol) was dissolved separately in 1mL DMF. After sonification for 1min the solutions were mixed, transferred into a Teflon vessel (25cm3) and heated in an autoclave at 393K for 48h. After cooling to room temperature the product was isolated by decanting the mother liquor and washed with DMF. For elemental analysis and TGA the product was dried under argon at room temperature for 6h. Yield 89% (based on 1,3-<strong>[69506-91-8]bib</strong>). Elemental analysis Calc. (%) for C24H16O4N4Co (Co(1,3-<strong>[69506-91-8]bib</strong>)(2,6-ndc)(DMF)1.5(H2O)1.5): C 55.21; H 4.8; N 12.43. Found: C 55.01; H 4.54; N 12.81.
  • 23
  • cobalt(II) nitrate hexahydrate [ No CAS ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • [ 787-70-2 ]
  • [ 33513-42-7 ]
  • [Co(1,3-bis(imidazol-1-yl)benzene)(4,4′-biphenyldicarboxylate)3](DMF)2(H2O) [ No CAS ]
YieldReaction ConditionsOperation in experiment
81% In N,N-dimethyl-formamide; at 119.84℃; for 48h;Autoclave; Co(NO3)2·6H2O (52.4mg, 0.2mmol) and H2(4,4′-bpdc) (48.4mg, 0.2mmol) were dissolved in 23mL DMF. 1,3-<strong>[69506-91-8]bib</strong> (31.5mg, 0.15mmol) was dissolved separately in 2mL DMF. After sonification for 1min the solutions were mixed, transferred into a Teflon vessel (50cm3) and heated in an autoclave at 393K for 48h. After cooling to room temperature the product was isolated by decanting the mother liquor and washed with DMF. For elemental analysis and TGA the product was dried under argon at room temperature for 6h. Yield 64% (based on H2(4,4′-bpdc)). Elemental analysis Calc. (%) for C57H41O13N5Co3 (Co3(1,3-<strong>[69506-91-8]bib</strong>)(4,4′-bpdc)3(DMF)2(H2O)): C 56.30; H 4.27; N 7.29. Found: C 55.94; H 4.01; N 7.65.
  • 24
  • [ 7766-51-0 ]
  • [ 69506-91-8 ]
  • 1,3-bis(3′-but-3″-enyl-imidazolium-3′-yl)benzene diiodide [ No CAS ]
  • 25
  • [ 7766-48-5 ]
  • [ 69506-91-8 ]
  • 1,3-bis(3′-pent-4″-enyl-imidazolium-3′-yl)benzene diiodide [ No CAS ]
  • 26
  • [ 4860-03-1 ]
  • [ 69506-91-8 ]
  • 1,3-bis(3-hexadecylimidazolium)benzene dichloride [ No CAS ]
  • 27
  • [ 7681-65-4 ]
  • [ 69506-91-8 ]
  • [Cu4I4(1,3-di(imidazol-1-yl)benzene)]n [ No CAS ]
  • 28
  • [ 7681-65-4 ]
  • [ 69506-91-8 ]
  • [Cu2I2(1,3-di(imidazol-1-yl)benzene)2]n [ No CAS ]
  • 29
  • [ 7681-65-4 ]
  • [ 69506-91-8 ]
  • [Cu4I4(1,3-di(imidazol-1-yl)benzene)3]n [ No CAS ]
  • 30
  • dodecatungstosilic acid [ No CAS ]
  • [ 7732-18-5 ]
  • cobalt(II) acetate [ No CAS ]
  • [ 69506-91-8 ]
  • [Co(H2O)2(1,3-bis(1-imidazoly)benzene)2]2[SiW12O40] [ No CAS ]
  • 31
  • 12-tungstoboric acid [ No CAS ]
  • [ 7732-18-5 ]
  • cobalt(II) acetate [ No CAS ]
  • [ 69506-91-8 ]
  • [Co2(H2O)(1,3-bis(1-imidazoly)benzene)4](HBW12O40).H2O [ No CAS ]
  • 32
  • ammonium metavanadate [ No CAS ]
  • [ 6147-53-1 ]
  • [ 69506-91-8 ]
  • Co(1,3-bis(1-imidazolyl)benzene)V<SUB>2</SUB>O<SUB>6</SUB> [ No CAS ]
  • 33
  • [ 69506-91-8 ]
  • 2-(1,3-bis(3-p-ter-tbutylphenylimidazol-2-ylidene)phenylene)(dimethylamido)triflate zirconium (IV) [ No CAS ]
  • 34
  • [ 69506-91-8 ]
  • 2-(1,3-bis(3-p-tert-butylphenylimidazol-2-ylidene)phenylene)(chloro) platinum (II) [ No CAS ]
  • 35
  • diphenyliodonium tetrafluoroborate [ No CAS ]
  • [ 69506-91-8 ]
  • 1,1'-(1,3-phenylene)bis(3-phenyl-1H-imidazol-3-ium) bis(tetrafluoroborate) [ No CAS ]
  • 36
  • [ 84563-54-2 ]
  • [ 69506-91-8 ]
  • 1,1'-(1,3-phenylene)bis(3-(4-(tert-butyl)phenyl)-1H-imidazol-3-ium) bis(trifluoromethanesulfonate) [ No CAS ]
  • 37
  • [ 732306-64-8 ]
  • [ 69506-91-8 ]
  • 1,1'-(1,3-phenylene)bis(3-(4-fluorophenyl)-1H-imidazol-3-ium) bis(trifluoromethanesulfonate) [ No CAS ]
  • 38
  • cobalt(II) chloride hexahydrate [ No CAS ]
  • [ 623904-16-5 ]
  • [ 69506-91-8 ]
  • [Co2(4,5-di(4′-carboxylphenyl)phthalic acid)(1,3-bis(imidazol-1-yl)benzene)]n [ No CAS ]
  • 39
  • nickel(II) chloride hexahydrate [ No CAS ]
  • 1,3-di(2′,4′-dicarboxyphenyl)benzene [ No CAS ]
  • [ 69506-91-8 ]
  • [Ni2(1,3-di(2',4'-dicarboxylphenyl)benzene)(1,3-bis(1H-imidazol-4-yl)benzene)22-H2O)]*2H2O [ No CAS ]
  • 40
  • platinum(II)-nitrate [ No CAS ]
  • [ 69506-91-8 ]
  • [Pt3(1,3-bis(1-imidazolyl)benzene)6](NO3)6 [ No CAS ]
  • 41
  • [ 69506-91-8 ]
  • 2-(diphenylphosphanyl)-1-{3-[2-(diphenylphosphanyl)-3-methyl-1H-imidazol-3-ium-1 yl]phenyl}-3-methyl-1H-imidazol-3-ium bistriflate [ No CAS ]
  • 42
  • [ 69506-91-8 ]
  • C37H27IrN4OP2 [ No CAS ]
  • 43
  • [ 69506-91-8 ]
  • C37H28ClIrN4OP2 [ No CAS ]
  • 44
  • [ 69506-91-8 ]
  • C39H34ClIrN4OP2(2+)*2CF3O3S(1-) [ No CAS ]
  • 45
  • [ 69506-91-8 ]
  • C36H28N4P2Se2 [ No CAS ]
  • 46
  • [ 69506-91-8 ]
  • 2CF3O3S(1-)*C38H34N4P2Se2(2+) [ No CAS ]
  • 47
  • [ 69506-91-8 ]
  • 1,3-bis(2-chloro-imidazol-1-yl)benzene [ No CAS ]
  • 48
  • silicotungstic acid hexahydrate [ No CAS ]
  • [ 7732-18-5 ]
  • [ 6018-89-9 ]
  • [ 69506-91-8 ]
  • [Ni2(1,3-bis(1-imidazolyl)benzene)4(H2O)4][SiW12O40] [ No CAS ]
YieldReaction ConditionsOperation in experiment
40% A mixture of H4SiW12O406H2O (302.1 mg, 0.1 mmol), bimb (109.4 mg, 0.51 mmol), Mn(CH3COO)24H2O(29.3 mg, 0.12 mmol), and H2O (15 mL) was stirred for1 h. The pH was adjusted to 4.6 with 1 M NaOH, and then the mixture was transferred to an 18-mL Teflon-lined reactor and kept under autogenous pressure at 160 C for4 days. After the reactor was slowly cooled to room temperature at a rate of 10 C/h, brownish block crystals were obtained. The crystals were collected, washed with distilled water, and dried at room temperature (39 % yield based on W). Elemental analysis for C72H70MnN24O82Si2W24 (1)(7106.71): Anal. Calc.: C, 12.17; H, 0.95; N, 4.73; Mn,0.77; W, 62.11 (%). Found: C, 12.69; H, 1.12; N, 4.91; Mn,0.71; W, 61.41 (%).
  • 49
  • silicotungstic acid hexahydrate [ No CAS ]
  • [ 7732-18-5 ]
  • [ 6156-78-1 ]
  • [ 69506-91-8 ]
  • [Mn(H2O)2(1,3-bis(1-imidazolyl)benzene)2(H3SiW12O40)2](1,3-bis(1-imidazolyl)benzene)4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
39% A mixture of H4SiW12O406H2O (302.1 mg, 0.1 mmol), bimb (109.4 mg, 0.51 mmol), Mn(CH3COO)24H2O(29.3 mg, 0.12 mmol), and H2O (15 mL) was stirred for1 h. The pH was adjusted to 4.6 with 1 M NaOH, and then the mixture was transferred to an 18-mL Teflon-lined reactor and kept under autogenous pressure at 160 C for4 days. After the reactor was slowly cooled to room temperature at a rate of 10 C/h, brownish block crystals were obtained. The crystals were collected, washed with distilled water, and dried at room temperature (39 % yield based on W). Elemental analysis for C72H70MnN24O82Si2W24 (1)(7106.71): Anal. Calc.: C, 12.17; H, 0.95; N, 4.73; Mn,0.77; W, 62.11 (%). Found: C, 12.69; H, 1.12; N, 4.91; Mn,0.71; W, 61.41 (%).
  • 50
  • silicotungstic acid hexahydrate [ No CAS ]
  • [ 7732-18-5 ]
  • [ 5970-45-6 ]
  • [ 69506-91-8 ]
  • [Zn2(1,3-bis(1-imidazolyl)benzene)4(H2O)4][SiW12O40] [ No CAS ]
YieldReaction ConditionsOperation in experiment
44% General procedure: A mixture of H4SiW12O406H2O (302.1 mg, 0.1 mmol), bimb (109.4 mg, 0.51 mmol), Mn(CH3COO)24H2O(29.3 mg, 0.12 mmol), and H2O (15 mL) was stirred for1 h. The pH was adjusted to 4.6 with 1 M NaOH, and then the mixture was transferred to an 18-mL Teflon-lined reactor and kept under autogenous pressure at 160 C for4 days. After the reactor was slowly cooled to room temperature at a rate of 10 C/h, brownish block crystals were obtained. The crystals were collected, washed with distilled water, and dried at room temperature (39 % yield based on W).
  • 51
  • copper(II) choride dihydrate [ No CAS ]
  • hexaammonium heptamolybdate tetrahydrate [ No CAS ]
  • [ 69506-91-8 ]
  • 4C12H10N4*Mo8O26(4-)*2Cu(2+) [ No CAS ]
  • 52
  • [ 638-45-9 ]
  • [ 69506-91-8 ]
  • 1,3-bis(3-hexylimidazol-3-ium-1-yl)benzene diiodide [ No CAS ]
YieldReaction ConditionsOperation in experiment
82% In acetonitrile; at 120℃; for 1h;Inert atmosphere; 1,3-Bis(imidazol-1'-yl)benzene (1) (3.12 g, 14.7 mmol),1-iodohexane (45.0 mL, 305 mmol), and CH3CN (100 mL) werecombined in air, degassed, and heated at 120 C for 1 h. The reaction was cooled to room temperature, and concentrated under vacuum yielding a yellow solid. The solid was washedonto a frit with 1 : 1 CH3CN/Et2O (50 mL) and washed withadditional 1 : 1 CH3CN/Et2O (250 mL). The resulting whitesolid (7.64 g, 82 %) was dried under vacuum at 110 C overnight.dH (DMSO-d6) 10.01 (s, 2H), 8.45 (s, 2H), 8.38 (s, 1H), 8.15(s, 2H), 8.05-7.98 (m, 3H), 4.30 (t, 4H, J 7.3), 1.93 (m, 4H),1.315 (m, 12H), 0.87 (t, 6H, J 6.6). dC (DMSO-d6) 135.7, 135.6,131.9, 123.5, 122.6, 121.0, 115.7, 49.6, 30.5, 29.0, 25.1, 21.8,13.8; HRMS m/z 507.1965 [MI], calcd for C24H36IN4507.1979; 379.2847 [M2IH], calcd for C24H35N4379.2856.
  • 53
  • [ 4282-44-4 ]
  • [ 69506-91-8 ]
  • 1,3-bis(3-undecylimidazol-3-ium-1-yl)benzene diiodide [ No CAS ]
YieldReaction ConditionsOperation in experiment
75% In acetonitrile; at 90℃; for 5.5h;Inert atmosphere; 1-iodoundecane (5.055 g, 17.91 mmol), and CH3CN (5 mL)were combined in air, degassed, and heated at 90 C for 5.5 h. During this time, white crystals formed. The reaction was allowed to cool to room temperature. The crystals were collected,washed with acetonitrile (210mL) and hexane (510mL),and dried under vacuum at 150 C for 24 h (3.429 g, 75 %).dH (DMSO-d6) 10.06 (s, 2H), 8.48 (s, 2H), 8.41 (s, 1H), 8.17 (s,2H), 8.07-7.95 (m, 3H), 4.31 (t, 4H, J 7.1), 1.93 (m, 4H), 1.32-1.23 (m, 34H), 0.84 (t, 6H, J 6.6). dC (DMSO-d6) 135.63, 135.58,131.9, 123.5, 122.5, 121.0, 115.6, 49.6, 31.2, 29.0, 28.9, 28.7,28.6, 28.3, 25.5, 22.0, 13.9. HRMS m/z 647.3553 [MI], calcdfor C34H56I4 647.3544.
  • 54
  • [ 69506-91-8 ]
  • [ 70145-42-5 ]
  • C40H48B2N8(2+)*2I(1-) [ No CAS ]
  • 55
  • [ 69506-91-8 ]
  • [ 62731-43-5 ]
  • C40H48B2N8(2+)*2CF3O3S(1-) [ No CAS ]
  • 56
  • [ 60669-69-4 ]
  • [ 69506-91-8 ]
  • C40H56B2N8(2+)*2CF3O3S(1-) [ No CAS ]
  • 57
  • [ 69506-91-8 ]
  • 9-(3-chloro-propyl)-9-bora-bicyclo[3.3.1]nonane [ No CAS ]
  • C40H48B2N8(2+)*2Cl(1-) [ No CAS ]
  • 58
  • [ 461441-22-5 ]
  • [ 69506-91-8 ]
  • C40H48B2N8(2+)*2Br(1-) [ No CAS ]
  • 59
  • copper(ll) sulfate pentahydrate [ No CAS ]
  • [ 69506-91-8 ]
  • Cu(2+)*O4S(2-)*2H2O*2C12H10N4 [ No CAS ]
  • 60
  • palladium (II) nitrate [ No CAS ]
  • [ 1258947-79-3 ]
  • 1,3-bis((E)-2-(pyridin-3-yl)vinyl)benzene [ No CAS ]
  • [ 69506-91-8 ]
  • [Pd6(tris[4-(1H-imidazol-1-yl)phenyl]amine)8(NO3)12] [ No CAS ]
  • 61
  • palladium (II) nitrate [ No CAS ]
  • [ 1258947-79-3 ]
  • [ 69506-91-8 ]
  • [Pd3(1,3-di(1H-imidazol-1-yl)benzene)6(NO3)6] [ No CAS ]
  • 62
  • palladium (II) nitrate [ No CAS ]
  • [ 69506-91-8 ]
  • [Pd3(1,3-di(1H-imidazol-1-yl)benzene)6(NO3)6] [ No CAS ]
  • 63
  • [ 499-81-0 ]
  • nickel(II) nitrate hexahydrate [ No CAS ]
  • [ 69506-91-8 ]
  • [ 33513-42-7 ]
  • [Ni2(μ3-OH)(μ2-NO3)(1,3-bis(1-imidazolyl)benzene)(3,5-pyridinedicarboxylate)]*xDMF [ No CAS ]
  • 64
  • [ 52462-29-0 ]
  • [ 69506-91-8 ]
  • [ 7681-11-0 ]
  • C44H48Cl2N8Ru2(2+)*2I(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
54.7% Under an argon atmosphere,0.06 mmol of dichloro (p-cymene) ruthenium (II) dimer was dissolved in chloroform,Made of the initial solution;0.2 mmol of 1,3-bis (1H-imidazol-1-yl) benzene 1,3-<strong>[69506-91-8]bib</strong>The ligand was added to a solution of dichloroaryl ruthenium dimer in chloroform, the reaction 10h at 60 C, to the reaction solution was added 1mmol of the desired anionic salt KI, stirred at room temperature for 48h; filtered and the filtrate was concentrated,The crude product was isolated and purified by column chromatography to give the dinitronuclear ruthenium complex 2 as a yellow powder with a yield of 54.7%.
  • 65
  • [ 14104-20-2 ]
  • [ 52462-29-0 ]
  • [ 69506-91-8 ]
  • C44H48Cl2N8Ru2(2+)*2BF4(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
80.3% Under an argon atmosphere,0.06 mmol of dichloro (p-cymene) ruthenium (II) dimer was dissolved in methanol,To make an initial solution; 0.6 mmol of 1,3-bis (1H-imidazol-1-yl) benzene 1,3-<strong>[69506-91-8]bib</strong>The ligand was added to a solution of dichloroaryl ruthenium dimer in methanol,After reaction at 70 C. for 40 h, 1 mmol of the desired anion salt AgBF 4 was added to the reaction solution,Stirred at room temperature for 2h; filtered and the filtrate was concentrated. The crude product was purified by column chromatography,To obtain a yellow powder binuclear aryl ruthenium metal complex 4, a yield of 80.3%,
  • 66
  • [ 26042-63-7 ]
  • [ 52462-29-0 ]
  • [ 69506-91-8 ]
  • C44H48Cl2N8Ru2(2+)*2F6P(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
89.2% Under an argon atmosphere,0.05 mmol of dichloro (p-cymene) ruthenium (II) dimer was dissolved in ethanol,Made of the initial solution;1.0 mmol of 1,3-bis (1H-imidazol-1-yl) benzene 1,3-<strong>[69506-91-8]bib</strong> ligand was added to a solution of dichloroaryl ruthenium dimer in ethanol and reacted at 80 C for 30 hours. To the reaction solution Add 1 mmol of the desired anionic salt AgPF6,Stirred at room temperature for 16h; filtered and the filtrate was concentrated. The crude product was purified by column chromatography,The yellow powder binuclear aromatic ruthenium metal complex 5 was obtained in a yield of 89.2%.
  • 67
  • [ 52462-29-0 ]
  • [ 2923-28-6 ]
  • [ 69506-91-8 ]
  • C44H48Cl2N8Ru2(2+)*2CF3O3S(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
92.1% Under an argon atmosphere,0.06 mmol of dichloro (p-cymene) ruthenium (II) dimer was dissolved in acetonitrile,To prepare an initial solution; 0.4 mmol of 1,3-bis (1H-imidazol-1-yl) benzene 1,3-<strong>[69506-91-8]bib</strong>The ligand was added to a solution of dichloroaryl ruthenium dimer in acetonitrile,After reacting for 72h at 80 C, 1 mmol of the desired anionic salt AgCF3SO3 was added to the reaction mixture,Stirred at room temperature for 4h; filtered and the filtrate was concentrated. The crude product was purified by column chromatography,The yellow powder binuclear aromatic ruthenium metal complex 1 was obtained in a yield of 92.1%.
  • 68
  • [ 52462-29-0 ]
  • silver nitrate [ No CAS ]
  • [ 69506-91-8 ]
  • C44H48Cl2N8Ru2(2+)*2NO3(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
55.4% Under an argon atmosphere,0.2 mmol of dichloro (p-cymene) ruthenium (II) dimer was dissolved in methylene chloride,Made of the initial solution;0.05 mmol of 1,3-bis (1H-imidazol-1-yl) benzene 1,3-<strong>[69506-91-8]bib</strong> ligand was added to a solution of dichloroaryl ruthenium dimer in dichloromethane, and after reaction at 25 C for 24 h,1 mmol of the desired anionic salt of AgNO 3 was added to the reaction mixture and stirred at room temperature for 24 h. The mixture was filtered and the filtrate was concentrated. The crude product was separated and purified by column chromatography to obtain a yellow powder binuclear aromatic ruthenium complex 3,The yield was 55.4%.
  • 69
  • zinc(II) nitrate hexahydrate [ No CAS ]
  • [ 7500-53-0 ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • [Zn(opda)(1,3-bis(1-imidazoly)benzene)]*H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
With potassium hydroxide; at 150℃; for 72.0h;Autoclave; High pressure; General procedure: A mixture of opda (0.0096g, 0.05mmol), Zn(NO3)2·6H2O (0.0297g, 0.1mmol), obiyb (0.0238g, 0.1mmol) and KOH (0.056g, 0.1mmol) were added to water (12mL) in a 25mL Teflon-lined stainless steel vessel. The mixture was heated at 150C for 72h. After the reactive mixture was slowly cooled to room temperature, colourless block crystals of 1 were obtained. Elemental analysis calcd. (%) for C24H22N4O4Zn: C 58.13, H 4.47, N 11.29; found (%): C 53.08, H 4.40, N 11.15.
  • 70
  • cadmium(II) sulfate octahydrate [ No CAS ]
  • N,N'-dioxide 3,3'-benzo(c)cinnolinedicarboxylic acid [ No CAS ]
  • [ 69506-91-8 ]
  • C14H6N2O6(2-)*Cd(2+)*C12H10N4*2H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
48% With sodium hydroxide; In water; at 130℃; for 72h;High pressure; Autoclave; A mixture of H2DBCD (0.17 mmol, 0.050 g), 1,3-<strong>[69506-91-8]bib</strong> (0.30 mmol,0.063 g), CdSO4·8H2O (0.20 mmol, 0.070 g), NaOH (0.30 mmol, 0.012g) and 9 mL H2O was placed in a Teflon-lined stainless steel vessel,heated to 130 C for 3 days, followed by slow cooling (a descent rate of10 oC/h) to room temperature. Light yellow block crystals of 1 were obtained. Yield of 48% (based on Cd). Anal. (%) calcd. forC26H22CdN6O8: C, 47.39; H, 3.67; N, 12.75. Found: C, 48.11; H,3.23; N, 12.69.
  • 71
  • [ 29089-56-3 ]
  • [ 69506-91-8 ]
  • [Pd2(2,2′-bipyridyl)2(1,3-bis(1-imidazolyl)benzene)2](NO3)4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
94% In water; acetonitrile; for 0.25h; General procedure: The ligand L (20mg, 0.093mmol) was added to the yellow-coloured solution of Pd(en)(NO3)2 (27mg, 0.093mmol) in acetonitrile-water (1:1) (5mL). The resulting clear solution was stirred for 8h, followed by complete evaporation of the solvent. The residual mass was dried under vacuum to afford the complex 1 as an off-white powder. The other complexes, [Pd2(tmeda)2(L)2](NO3)4, 2, [Pd2(bpy)2(L)2](NO3)4, 3, and [Pd2(phen)2(L)2](NO3)4, 4, were prepared in a similar manner by using appropriate cis-protected palladium(II) components. The complex [Pd2(phen)2(L)2](OTf)4, 4′ was prepared using Pd(phen)(OTf)2 as the metal component. The reactions mixtures were stirred for 2h to prepare the complex 2 and for 15min to prepare the complexes 3, 4 and 4′.
  • 72
  • [ 31476-92-3 ]
  • [ 69506-91-8 ]
  • [Pd2(1,10-phenanthroline)2(1,3-bis(1-imidazolyl)benzene)2](NO3)4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
95% In water; acetonitrile; for 0.25h; General procedure: The ligand L (20mg, 0.093mmol) was added to the yellow-coloured solution of Pd(en)(NO3)2 (27mg, 0.093mmol) in acetonitrile-water (1:1) (5mL). The resulting clear solution was stirred for 8h, followed by complete evaporation of the solvent. The residual mass was dried under vacuum to afford the complex 1 as an off-white powder. The other complexes, [Pd2(tmeda)2(L)2](NO3)4, 2, [Pd2(bpy)2(L)2](NO3)4, 3, and [Pd2(phen)2(L)2](NO3)4, 4, were prepared in a similar manner by using appropriate cis-protected palladium(II) components. The complex [Pd2(phen)2(L)2](OTf)4, 4′ was prepared using Pd(phen)(OTf)2 as the metal component. The reactions mixtures were stirred for 2h to prepare the complex 2 and for 15min to prepare the complexes 3, 4 and 4′.
  • 73
  • Pd(1,10-phenanthroline)(OTf)<SUB>2</SUB> [ No CAS ]
  • [ 69506-91-8 ]
  • [Pd2(1,10-phenanthroline)2(1,3-bis(1-imidazolyl)benzene)2](OTf)4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
95% In water; acetonitrile; for 0.25h; General procedure: The ligand L (20mg, 0.093mmol) was added to the yellow-coloured solution of Pd(en)(NO3)2 (27mg, 0.093mmol) in acetonitrile-water (1:1) (5mL). The resulting clear solution was stirred for 8h, followed by complete evaporation of the solvent. The residual mass was dried under vacuum to afford the complex 1 as an off-white powder. The other complexes, [Pd2(tmeda)2(L)2](NO3)4, 2, [Pd2(bpy)2(L)2](NO3)4, 3, and [Pd2(phen)2(L)2](NO3)4, 4, were prepared in a similar manner by using appropriate cis-protected palladium(II) components. The complex [Pd2(phen)2(L)2](OTf)4, 4′ was prepared using Pd(phen)(OTf)2 as the metal component. The reactions mixtures were stirred for 2h to prepare the complex 2 and for 15min to prepare the complexes 3, 4 and 4′.
  • 74
  • [ 63994-76-3 ]
  • [ 69506-91-8 ]
  • [Pd2(ethylenediamine)2(1,3-bis(1-imidazolyl)benzene)2](NO3)4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
93% In water; acetonitrile; at 20℃; for 8h; The ligand L (20mg, 0.093mmol) was added to the yellow-coloured solution of Pd(en)(NO3)2 (27mg, 0.093mmol) in acetonitrile-water (1:1) (5mL). The resulting clear solution was stirred for 8h, followed by complete evaporation of the solvent. The residual mass was dried under vacuum to afford the complex 1 as an off-white powder. The other complexes, [Pd2(tmeda)2(L)2](NO3)4, 2, [Pd2(bpy)2(L)2](NO3)4, 3, and [Pd2(phen)2(L)2](NO3)4, 4, were prepared in a similar manner by using appropriate cis-protected palladium(II) components. The complex [Pd2(phen)2(L)2](OTf)4, 4′ was prepared using Pd(phen)(OTf)2 as the metal component. The reactions mixtures were stirred for 2h to prepare the complex 2 and for 15min to prepare the complexes 3, 4 and 4′. 2.5. Analytical data; 1: 1H NMR (400MHz, DMSO-d6): δ = 9.54 (s, 4H, Ha), 8.92 (s,2H, Hb), 8.74 (t, J=1.6Hz, 2H, Hc), 8.36 (t, J=5.2Hz, 6H, Hd, He), 8.03 (t, J=1.6Hz, 2H, Hf), 6.18 (s, 4H, Hg), and 3.25 (s, 4H, Hh). 13C NMR (100MHz, DMSO-d6): δ = 137.3, 136.5, 131.8, 129.9, 120.5, 120.0, 114.6 and 46.9ppm. Yield: (44mg, 93%). MP - 235C (decomposed). ESI-MS: m/z=271 which correspond to [1 - 3NO3]
  • 75
  • [ 761442-02-8 ]
  • [ 69506-91-8 ]
  • [Pd2(tetramethylethylenediamine)2(1,3-bis(1-imidazolyl)benzene)2](NO3)4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
93% In water; acetonitrile; for 2h; General procedure: The ligand L (20mg, 0.093mmol) was added to the yellow-coloured solution of Pd(en)(NO3)2 (27mg, 0.093mmol) in acetonitrile-water (1:1) (5mL). The resulting clear solution was stirred for 8h, followed by complete evaporation of the solvent. The residual mass was dried under vacuum to afford the complex 1 as an off-white powder. The other complexes, [Pd2(tmeda)2(L)2](NO3)4, 2, [Pd2(bpy)2(L)2](NO3)4, 3, and [Pd2(phen)2(L)2](NO3)4, 4, were prepared in a similar manner by using appropriate cis-protected palladium(II) components. The complex [Pd2(phen)2(L)2](OTf)4, 4′ was prepared using Pd(phen)(OTf)2 as the metal component. The reactions mixtures were stirred for 2h to prepare the complex 2 and for 15min to prepare the complexes 3, 4 and 4′.
  • 76
  • [ 52462-29-0 ]
  • [ 64-17-5 ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • [Ru(η6-p-cymene)(1,3-di(1H-imidazol-1-yl)benzene)Cl]2Cl2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
85.4% for 12h;Inert atmosphere; Reflux; The ligand 1,3-<strong>[69506-91-8]bib</strong>(42.0 mg, 0.2 mmol) was added to a 20 mL ethanol solution ofRu2(η6-p-cymene)2Cl4 (61.2 mg, 0.1 mmol). After refluxing for 12 hunder N2 protection, the solvent was removed and the crude productwas further purified by silica gel chromatography with CH2Cl2/CH3OH.The sample was recrystallized by dissolving with CH2Cl2 and petroleumether was added as an anti-solvent. A pale yellow product was collected with a yield of 92.8 mg (ca. 85.4% based on the consumed Ru(II)dimer). Elemental analysis: calcd (%) forRu2C44H48N8Cl4·C2H5OH·0.5(H2O): C, 50.78; H, 5.10; N, 10.30.Found: C, 50.82; H, 5.19; N, 10.39. 1H NMR (DMSO-d6, 400 MHz):10.37 (4H, s, Him), 9.09 (2H, s, Hbz, 1,3-<strong>[69506-91-8]bib</strong>), 8.11 (4H, t, Him), 7.80 (4H,dd, J=7.0, J=1.9 Hz, Hbz, 1,3-<strong>[69506-91-8]bib</strong>), 7.74 (2H, dd, J=9.4, J=6.6 Hz,Hbz, 1,3-<strong>[69506-91-8]bib</strong>), 7.50 (4H, s, Hbz, 1,3-<strong>[69506-91-8]bib</strong>), 6.09 (8H, dd, J=18.0,J=6.1 Hz, Hbz, p-cymene), 2.57 (2H, s, CH), 1.84 (6H, s, CH3), 1.16(12H, d, J=6.9 Hz, CH3). ESI-MS(+): calcd. For [1-Cl-]+ m/z:997.42, found m/z 998.92.
  • 77
  • [ 280-57-9 ]
  • Cu<SUB>4</SUB>(1,3-phenylenebis(azanetriyl)tetrabenzoate)<SUB>2</SUB> [ No CAS ]
  • [ 69506-91-8 ]
  • Cu4(1,3-phenylenebis(azanetriyl)tetrabenzoate)2(1,3-bis(1H-imidazol-1-yl)benzene)0.5(1,4-diazabicyclo[2.2.2]octane)1.85 [ No CAS ]
YieldReaction ConditionsOperation in experiment
General procedure: To the washed crystals of DUT-71, 1,3-<strong>[69506-91-8]bib</strong>, chir-R-1,3-<strong>[69506-91-8]bib</strong>, or chir-S-1,3-<strong>[69506-91-8]bib</strong> (0.34 mmol) dissolved in a mixture of DMF and ethanol (1:1, 6 ml), was added and heated to 80C for 7 days. After cooling down to room temperature the supernatant was replaced with a fresh mixture of DMF and ethanol (1:1). To the resulted, 1,3-<strong>[69506-91-8]bib</strong> containing compound, dabco (57.4 mg, 0.51 mmol) dissolved in a mixture of DMF and ethanol (1:1, 6 ml), was added and the mixture was heated to 80C for 7 days. After cooling down to room temperature the solvent was replaced with a fresh mixture of DMF and ethanol (1:1). Elemental analysis for DUT-90: Cu4(C68O16N4H40)(C12N4H10)0.5(C6N2H12)1.85(C2H6O)(H2O)2.9 [Cu4(mpbatb)2(1,3-<strong>[69506-91-8]bib</strong>)0.5(dabco)1.85(EtOH)(H2O)2.9]: calc. (%) C 57.0, H 4.3, N 7.4, found (%) C 57.1, H 4.4, N 7.2.
  • 78
  • [ 2855-08-5 ]
  • [ 69506-91-8 ]
  • 1,1'-(1,3-phenylene)bis(3-(3,3-dimethylbutyl)-1H-imidazol-3-ium) dichloride [ No CAS ]
YieldReaction ConditionsOperation in experiment
31% With sodium iodide; In acetonitrile; at 190℃; for 480h;Inert atmosphere; Glovebox; 1,1'-(1,3-phenylene)bis(3-(3,3-dimethylbutyl)-1H-imidazol-3-ium) dichloride (7) <strong>[69506-91-8]1,3-di(1H-imidazol-1-yl)benzene</strong> (1) (500 mg, 2.38 mmol), 1-chloro-3,3-dimethylbutane (1.7 mL, 11.9 mmol), sodium iodide (10 mg, 0.07 mmol) and MeCN (15 mL) were combined in a storage flask. The mixture was degassed with N2 gas for 3 min and heated at 190 C. in a closed system. After heating for 20 days, the mixture was transferred to a round-bottom flask. Solvent was removed under reduced pressure, yielding a brownish solid. The brownish solid was purified with silica gel chromatography (DCM/MeOH=9:1), yielding an off-white solid (330 mg, 31%). 1H NMR (300 MHz, DMSO-d6): 10.73 (s, 2H), 8.79 (s, 3H), 8.20 (s, 2H), 8.09 (d, 2H, J=8.0 Hz), 7.94 (t, 1H, J=8.1 Hz), 4.34 (t, 4H, J=8.3 Hz), 1.92 (t, 4H, J=8.1 Hz), 1.00 (s, 18H). 13C NMR (126 MHz, DMSO-d6): δ 136.6, 136.3, 132.4, 124.1, 122.1, 121.3, 115.3, 47.1, 43.2, 30.3, 29.5. HRMS (ESI) m/z 415.2426 ([M-Cl-]+ calcd for C24H36ClN4: 415.2623).
  • 79
  • zinc(II) sulfate heptahydrate [ No CAS ]
  • [ 14900-61-9 ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • C12H10N4*C16H13NO4(2-)*Zn(2+)*H2O [ No CAS ]
  • 80
  • [ 74-96-4 ]
  • [ 69506-91-8 ]
  • C16H20N4(2+)*2Br(1-) [ No CAS ]
  • 81
  • [ 69506-91-8 ]
  • [ 106-95-6 ]
  • C18H20N4(2+)*2Br(1-) [ No CAS ]
  • 82
  • zinc tetrafluoroborate [ No CAS ]
  • (S)-2-(4-acetylphenoxy)propionic acid [ No CAS ]
  • [ 69506-91-8 ]
  • C10H8O5(2-)*Zn(2+)*H2O*C12H10N4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
30% With 1,4-pyrazine; In N,N-dimethyl acetamide; water; at 90℃; for 72h; General procedure: Complex 1-D was synthesized by stirring Zn(BF4)2 (35 mg,0.15 mmol), (R)-H2CBA(21 mg, 0.1 mmol), 1,3-DIB (21 mg, 0.1 mmol) and pyrazine (96 mg, 1.2 mmol) in 6 ml of N,N-dimethylacetamide/water (1:3) solvent. The resulting mixture was placed in a 23mL Teflon reactor and kept under autogenous pressure at 90 C for three days. After slowly being cooled to room temperature, colorless crystals were filteredand washed with ethanol and dried in the air.
  • 83
  • zinc tetrafluoroborate [ No CAS ]
  • (S)-2-(4-acetylphenoxy)propionic acid [ No CAS ]
  • [ 69506-91-8 ]
  • 2C10H8O5(2-)*2Zn(2+)*2C12H10N4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
50% With 1,4-pyrazine; In N,N-dimethyl acetamide; water; at 120℃; for 72h; General procedure: Complex 1-D was synthesized by stirring Zn(BF4)2 (35 mg,0.15 mmol), (R)-H2CBA(21 mg, 0.1 mmol), 1,3-DIB (21 mg, 0.1 mmol) and pyrazine (96 mg, 1.2 mmol) in 6 ml of N,N-dimethylacetamide/water (1:3) solvent. The resulting mixture was placed in a 23mL Teflon reactor and kept under autogenous pressure at 90 C for three days. After slowly being cooled to room temperature, colorless crystals were filteredand washed with ethanol and dried in the air.
  • 84
  • (R)-2-(4-acetylphenoxy)propionic acid [ No CAS ]
  • zinc tetrafluoroborate [ No CAS ]
  • [ 69506-91-8 ]
  • C10H8O5(2-)*Zn(2+)*H2O*C12H10N4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
40% With 1,4-pyrazine; In N,N-dimethyl acetamide; water; at 90℃; for 72h; Complex 1-D was synthesized by stirring Zn(BF4)2 (35 mg,0.15 mmol), (R)-H2CBA(21 mg, 0.1 mmol), 1,3-DIB (21 mg, 0.1 mmol) and pyrazine (96 mg, 1.2 mmol) in 6 ml of N,N-dimethylacetamide/water (1:3) solvent. The resulting mixture was placed in a 23mL Teflon reactor and kept under autogenous pressure at 90 C for three days. After slowly being cooled to room temperature, colorless crystals were filteredand washed with ethanol and dried in the air. Yield: 40% (based on (R)-H2CBA). Anal. Calcd. for C22H20N4O6Zn (%): C, 52.66; H, 4.02; N, 11.17.Found (%): C, 50.24; H, 3.62; N, 9.84. IR (KBr, cm1): 3345.8(w),3137.0(w),1603.5(s), 1558.0(m), 1512.1(s), 1381.5(s), 1283.7(m),1231.4(s), 1179.5(m), 1055.4(s), 944.4(w), 853.3(w), 787.8(m),735.6(w), 657.3(m), 494.4(w).
  • 85
  • (R)-2-(4-acetylphenoxy)propionic acid [ No CAS ]
  • zinc tetrafluoroborate [ No CAS ]
  • [ 69506-91-8 ]
  • 2C10H8O5(2-)*2Zn(2+)*2C12H10N4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
50% With 1,4-pyrazine; In N,N-dimethyl acetamide; water; at 120℃; for 72h; General procedure: Complex 1-D was synthesized by stirring Zn(BF4)2 (35 mg,0.15 mmol), (R)-H2CBA(21 mg, 0.1 mmol), 1,3-DIB (21 mg, 0.1 mmol) and pyrazine (96 mg, 1.2 mmol) in 6 ml of N,N-dimethylacetamide/water (1:3) solvent. The resulting mixture was placed in a 23mL Teflon reactor and kept under autogenous pressure at 90 C for three days. After slowly being cooled to room temperature, colorless crystals were filteredand washed with ethanol and dried in the air.
  • 86
  • zinc(II) nitrate hexahydrate [ No CAS ]
  • [ 100-21-0 ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • [Zn(1,4-dicarboxylatobenzene)(1,3-bis(imidazol-1-yl)benzene)](H2O)3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
62% In methanol; N,N-dimethyl-formamide; at 85℃; for 120h; For complex 1, a mixture of <strong>[69506-91-8]bib</strong> (21.2 mg, 0.1 mmol), H2bdc(17 mg, 0.1 mmol) and Zn(NO3)2 6H2O (29.7 mg, 0.1 mmol)were dissolved in 5mL of DMF-MeOH-H2O (3/1/1) solventin a Glass vial (10 mL) and stirred for 30 min. The vesselwas placed in an oven and heated at 85 C for 5 days. Andthen the reaction mixture was cooled to room temperature.Colorless block crystals of 1 were isolated by filtration,washed with EtOH, and dried in air. The yield is about 62%yield (14.01 mg) based on the <strong>[69506-91-8]bib</strong> ligand. Anal. Calcd forC19H18N6O6Zn: C, 46.41; H, 3.69; N, 17.09; Found: C, 46.56;H, 3.78; N, 16.92.
  • 87
  • zinc(II) nitrate hexahydrate [ No CAS ]
  • [ 10312-55-7 ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • [Zn(2-amino-1,4-dicarboxylatobenzene)(1,3-bis(imidazol-1-yl)benzene)](H2O)3 [ No CAS ]
YieldReaction ConditionsOperation in experiment
48% In methanol; N,N-dimethyl-formamide; at 85℃; for 120h; For complex 2, a mixture of <strong>[69506-91-8]bib</strong> (21.2 mg, 0.1 mmol),NH2-H2bdc (19 mg, 0.1 mmol) and Zn(NO3)2 6H2O(29.7 mg, 0.1 mmol) were dissolved in 5mL of DMF-MeOHH2O(3/1/1) solvent in a Glass vial (10 mL) and stirred for30 min. The vessel was placed in an oven and heated at85 C for 5 days. And then the reaction mixture was cooledto room temperature. Yellow block crystals were isolated byfiltration, washed with EtOH, and dried in air. The yield isabout 48% yield (11.9 mg) based on the <strong>[69506-91-8]bib</strong> ligand. Anal.Calcd for C20H15N5O4Zn: C, 52.82; H, 3.32; N, 15.40;Found: C, 52.56; H, 3.78; N, 15.62.
  • 88
  • copper(II) nitrate trihydrate [ No CAS ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • [ 33513-42-7 ]
  • [ 1258-71-5 ]
  • 0.5C15H12N6O12(6-)*1.5Cu(2+)*5H2O*C3H7NO*1.5C12H10N4 [ No CAS ]
YieldReaction ConditionsOperation in experiment
Ca. 47% With nitric acid; at 80℃; for 72h;Autoclave; High pressure; A mixture of Cu(NO3)23H2O (24.2 mg, 0.1 mmol), bimb ligand (21.1 mg, 0.1 mmol), and H6L(47.4 mg, 0.1 mmol) were dissolved in DMF/H2O/0.1MHNO3 solvent (8:2:1, 11 mL). After being mixedevenly, it was placed in a Parr Teflon-lined stainless steel vessel (20 mL) and heated at 80 C for 72 hunder autogenous pressure. Aquamarine crystals were acquired. The reaction yield was ca. 47% basedon an H6L ligand. The elemental analysis for C57H64N20Cu3O24(%): C, 42.68; H, 4.02; N, 17.47. Found:C, 42.99; H, 4.12; N, 16.68. FT-IR (4000-400 cm1): 3736 (s), 3393 (s), 3130 (s), 1609 (m), 1517 (m), 1289(m), 1250 (m), 1194 (s), 1113 (s), 988 (s), 811 (s), 792 (s).
  • 89
  • cobalt(II) nitrate hexahydrate [ No CAS ]
  • [ 605-70-9 ]
  • [ 69506-91-8 ]
  • [ 68-12-2 ]
  • ([Co3(1,3-di(1H-imidazol-1-yl)benzene)2(1,4-naphthalenedicarboxylate)3]*2DMF)n [ No CAS ]
YieldReaction ConditionsOperation in experiment
40% In ethanol; at 90℃; for 72h;Sonication; Sealed tube; For complex 1, a mixture of Co(NO3)26H2O (29.7 mg,0.10 mmol), H2ndc (21.6 mg, 0.10 mmol) and dimb (21.0 mg,0.10 mmol) was dissolved in 6mL of mixed solvent of DMFand EtOH (v/v1:1) in a 10mL glass vial. After the mixturewas sonicated for 10 minutes, the vial was sealed andplaced in a 90 C oven for 3 days. Colorless block crystalswere obtained after cooling to room temperature in 24 h.The yield was about 40% based on Co(NO3)26H2O. Anal.Calcd for 1 (C66H50Co3N10O14): C, 57.28; H, 3.64; N,10.12%; Found for 1: C, 57.76; H, 3.23; N, 10.23%. IR (KBrpellet, cm1): 3420.4(w), 3111.2(w), 1639.3(s), 1597.1(s),1518.1(m), 1388.4(m), 1231.4(m), 1172.8(w), 1107.6(w),1062.2(m), 944.4(w), 786.4(m), 676.8(w), 654.9(w)(Figure S1).
  • 90
  • cobalt(II) nitrate hexahydrate [ No CAS ]
  • (R)-4-(1-carboxyethoxy)benzoic acid [ No CAS ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • ([Co2((R)-4-(1-carboxyethoxy)benzoate)2(1,3-di(1H-imidazol-1-yl)benzene)2](H2O))n [ No CAS ]
YieldReaction ConditionsOperation in experiment
40% With 1,4-pyrazine; In N,N-dimethyl acetamide; at 90℃; for 72h;Autoclave; High pressure; For complex 2, a mixture of Co(NO3)26H2O (29.7 mg,0.10 mmol), (R)-H2CBA(21 mg, 0.1 mmol), dimb (21.0 mg,0.10 mmol) and pyrazine (96 mg, 1.2 mmol) in 6 ml of N,Ndimethylacetamide/water (1:3) solvent. The resulting mixturewas placed in a 23 mL Teflon reactor and kept underautogenous pressure at 90 C for three days. After slowlybeing cooled to room temperature, colorless crystals werefiltered and washed with ethanol and dried in the air. Yield:40% (based on (R)-H2CBA). Anal. Calcd. for 2(C22H20N4O6Co, %): C, 52.66; H, 4.02; N, 11.17. Found (%):C, 50.24; H, 3.62; N, 9.84. IR (KBr pellet, cm1): 3437.2(w),3110.6(w), 1642.6(s), 1597.1(s), 1512.9(m), 1388.3(m),1231.4(m), 1172.8(w), 1140.1(w), 1062.2(m),944.4(w),787.8(m), 676.9(w), 657.3(w) (Figure S2).
  • 91
  • cadmium(II) nitrate tetrhydrate [ No CAS ]
  • [ 100-21-0 ]
  • [ 69506-91-8 ]
  • [ 33513-42-7 ]
  • C12H10N4*C8H4O4(2-)*Cd(2+)*C3H7NO*H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
30% In ethanol; water; at 120℃; for 48h;Autoclave; A 6 mL mixed solvent of DMF, H2Oand EtOH (v/v/v 4 : 1: 1) containing a mixture of Cd(NO3)24H2O (62mg, 0.2 mmol), <strong>[69506-91-8]bib</strong> (42 mg, 0.2 mmol), and H2bdc (17 mg, 0.1 mmol) wasstirred thoroughly, and transformed to a 23 mL Teflon-lined autoclave,which was then heated up to 120 C within 12 h and maintained for 36 h.After being cooled to room temperature in 24 h, colourless block crystalof 1 was collected. Yield: 30% (based on <strong>[69506-91-8]bib</strong> ligand). IR (KBr pellet,cm1): 3462 (w), 3128 (w), 1664 (s), 1608 (s), 1569 (m), 1513 (m), 1387(s), 1242 (s), 1118 (m), 1064 (m), 934 (w), 837 (m), 748 (s), 653 (m),527 (w).
  • 92
  • cadmium(II) nitrate tetrhydrate [ No CAS ]
  • [ 605-70-9 ]
  • [ 69506-91-8 ]
  • [ 68-12-2 ]
  • C12H10N4*C12H6O4(2-)*Cd(2+)*C3H7NO*H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
60% In ethanol; water; at 140℃; for 82h;Autoclave; A mixture of Cd(NO3)24H2O (62mg, 0.2 mmol), bib (42 mg, 0.2 mmol), and H2ndc (44 mg, 0.2 mmol) wasfirstly dissolved in 10 mL mixed solvent of DMF, H2O and EtOH (v/v/v 5 : 2: 3) under continuous stirring. Then, the as-obtained solution wassealed in a 23 mL Teflon-lined autoclave, and heated up to 140 C within10 h and maintained for 72 h. After being cooled to room temperature in24 h, colourless block crystal of 2 was collected. Yield: 60% (based on bibligand). IR (KBr pellet, cm1): 3430 (m), 1664 (s), 1615 (m), 1561 (s),1512 (s), 1394 (w), 1242 (m), 1121 (w), 1058 (m), 1104 (w), 931 (w),799 (m), 645 (m), 571 (w).
  • 93
  • cadmium(II) nitrate tetrhydrate [ No CAS ]
  • [ 69506-91-8 ]
  • [ 787-70-2 ]
  • 2C12H10N4*2C14H8O4(2-)*2Cd(2+)*1.5H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
30% In ethanol; water; N,N-dimethyl-formamide; at 160℃; for 82h;Autoclave; A mixture of Cd(NO3)24H2O (62mg, 0.2 mmol), <strong>[69506-91-8]bib</strong> (42 mg, 0.2 mmol), and H2bpdc (48 mg, 0.2 mmol) in8 mL mixed solvent of DMF, H2O and EtOH (v/v/v 4 : 2: 2) was sealedin a 23 mL Teflon-lined autoclave and stirred thoroughly, then heated upto 160 C within 10 h and maintained for 72 h. After being cooled toroom temperature in 24 h, colorless block crystal of 3 was collected.Yield: 30% (based on <strong>[69506-91-8]bib</strong> ligand). IR (KBr pellet, cm1): 3435 (w), 3126(w), 2360 (w), 1583 (m), 1516 (s), 1398 (s), 1243 (m), 1112 (w), 1064(w), 855 (w), 774 (s), 688 (w), 662 (w), 427 (w).
  • 94
  • cobalt(II) nitrate hexahydrate [ No CAS ]
  • (R)-4-(1-carboxyethoxy)benzoic acid [ No CAS ]
  • [ 69506-91-8 ]
  • C10H8O5(2-)*Co(2+)*1.5C12H10N4*0.5H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
30% With sodium carbonate; In water; at 140℃; for 72h; General procedure: The mixture of (R)-H2CBA (32 mg, 0.15 mmol), 2,5-DIP (36 mg, 0.15mmol), Na2CO3 (19 mg, 0.18 mmol), Co(NO3)2.6H2O (58 mg, 0.2 mmol)and H2O (6 mL) was added in a 23 mL teflon-lined stainless steel vessel and stired for 15 min. Then the vessel was sealed and heated to 140 C for three days. After cooling to room temperature, the red block crystals of 1 were obtained with a yield of 30% (based on (R)-H2CBA).
  • 95
  • zinc(II) nitrate hexahydrate [ No CAS ]
  • [ 121-91-5 ]
  • [ 69506-91-8 ]
  • C12H10N4*C8H4O4(2-)*Zn(2+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
62% In methanol; water; N,N-dimethyl-formamide; at 85℃; for 120h; For complex 1, a mixtureof <strong>[69506-91-8]bib</strong> (21.2 mg, 0.1 mmol), H2bdc (17 mg, 0.1 mmol), and Zn(NO3)26H2O (29.7 mg, 0.1 mmol) was dissolved in 5 mL ofa DMF-MeOH-H2O (3/1/1) solvent in a glass vial (10 mL) and stirred for 30 min. The vessel was placed in an oven andheated at 85 C for 5 days. And then the reaction mixture was cooled to room temperature. Colorless block crystals of 1 wereisolated by filtration, washed with EtOH, and dried in air. The yield was about 62% (14.01 mg) based on the <strong>[69506-91-8]bib</strong> ligand. Anal.calcd for C20H14N4O4Zn (%): C 54.63, H 3.21, N 12.74. Found (%): C 54.56, H 3.78, N 12.92.
  • 96
  • zinc(II) nitrate hexahydrate [ No CAS ]
  • [ 10312-55-7 ]
  • [ 69506-91-8 ]
  • [Zn(2-amino-1,4-dicarboxylatobenzene)(1,3-bis(imidazol-1-yl)benzene)] [ No CAS ]
YieldReaction ConditionsOperation in experiment
48% In methanol; water; N,N-dimethyl-formamide; at 85℃; for 120h; For complex 2, a mixture of <strong>[69506-91-8]bib</strong> (21.2 mg, 0.1 mmol), NH2-H2bdc (19 mg, 0.1 mmol), and Zn(NO3)26H2O(29.7 mg, 0.1 mmol) was dissolved in 5 mL of a DMF-MeOH-H2O (3/1/1) solvent in a glass vial (10 mL) and stirred for30 min. The vessel was placed in an oven and heated at 85 C for 5 days. And then the reaction mixture was cooled to roomtemperature. Yellow block crystals were isolated by filtration, washed with EtOH, and dried in air. The yield was about 48%(11.9 mg) based on the <strong>[69506-91-8]bib</strong> ligand. Anal. calcd for C20H15N5O4Zn (%): C 52.82, H 3.32, N 15.40. Found (%): C 52.56,H 3.78, N 15.62
  • 97
  • cobalt(II) nitrate hexahydrate [ No CAS ]
  • [ 677010-20-7 ]
  • [ 69506-91-8 ]
  • [Co2(1,3-di(1H-imidazol-1-yl)benzene)2(Hbpt)2]*H2O [ No CAS ]
YieldReaction ConditionsOperation in experiment
59% In ethanol; N,N-dimethyl-formamide; at 110℃; for 72h;Autoclave; For complex 2, a mixture of dimb (42.0 mg, 0.20 mmol), Co(NO3)2*6H2O (60 mg, 0.20 mmol), H3bpt (28.6 mg,0.1 mmol), and EtOH (0.5 mL) in DMF (8 mL) was sealed in a Teflon-lined stainless steel container and heated at 110 C for 3days. After being cooled to room temperature, pink block crystals of 2 were obtained in a 59% yield based on the dimb ligand.Anal. calcd for 2 (C42H28Co2N4O13) (%): C 55.16, H 3.09, Co 12.89, N 6.13. Found for 2 (%): C 55.27, H 3.12, N 6.01.
  • 98
  • cobalt(II) nitrate hexahydrate [ No CAS ]
  • [ 677010-20-7 ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • {Co3(1,3-di(1H-imidazol-1-yl)benzene)2(bpt)2(H2O)4}n [ No CAS ]
YieldReaction ConditionsOperation in experiment
67% With sodium hydroxide; at 120℃; for 72h;Autoclave; For complex 1, a mixture of dimb (21.0 mg, 0.10 mmol), Co(NO3)2*6H2O (60 mg, 0.20 mmol), H3bpt (28.6 mg, 0.1 mmol), and NaOH (12.0 mg, 0.3 mmol) in H2O (10 mL) was sealed in a Teflon-lined stainless steel container and heated at 120 C for 3 days. After being cooled to room temperature, pink block crystals of 1 were obtained in a 67% yield based on the dimbligand. Anal. calcd for 1 (C54H42Co3N8O16) (%): C 52.49, H 3.43, N 9.07. Found for 1 (%): C 52.76, H 3.23, N 5.23.
  • 99
  • 3,5-di(2’,4’-dicarboxylphenyl)benzoic acid [ No CAS ]
  • [ 7732-18-5 ]
  • [ 69506-91-8 ]
  • zinc(II) iodide [ No CAS ]
  • C23H9O10(5-)*1.5C12H10N4*H(1+)*3H2O*2Zn(1+) [ No CAS ]
YieldReaction ConditionsOperation in experiment
46% With sodium hydroxide; at 110℃; for 72h;Sealed tube; The starting reactants of 0.002 mmol H5DDB (0.9 mg), 0.006mmol <strong>[69506-91-8]bib</strong> (1.3 mg), and 0.006 mmol ZnI2 (1.9 mg), are added into1 mL DMA/dioxane/water (1:1:2) mixed solvents, and then onedrop 0.1 M NaOH is added into the mixed solvents to adjust thepH value. After transferring those suspensions in, the glass tubeis sealed in near vacuum by using the alcohol blowtorch. Thenthe sealed glass tube is heated at 110 C for 72 h, and followed acooling process with a 5 C/h to give birth to the single crystalsof 1, with a yield of 46 % (according to H5DDB). Calcd. (%) EA for1 (C41H31N6O13Zn2): C, 50.03; H, 3.30; N, 8.88, found (%): C,49.82; H, 3.43; N, 8.69. FT-IR (cm1): 3436 (vs), 2362 (s), 1620(vs), 1515 (s), 1375 (vs), 1118 (w), 1077 (m), 786 (m), 657 (w)(Fig. S1).
  • 100
  • cadmium(II) nitrate tetrhydrate [ No CAS ]
  • [ 7325-46-4 ]
  • [ 69506-91-8 ]
  • C12H10N4*H2O*Cd(2+)*C10H8O4(2-) [ No CAS ]
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