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CAS No. : | 2966-50-9 | MDL No. : | MFCD00013199 |
Formula : | C2AgF3O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | KZJPVUDYAMEDRM-UHFFFAOYSA-M |
M.W : | 220.88 | Pubchem ID : | 76299 |
Synonyms : |
|
Num. heavy atoms : | 8 |
Num. arom. heavy atoms : | 0 |
Fraction Csp3 : | 0.5 |
Num. rotatable bonds : | 1 |
Num. H-bond acceptors : | 5.0 |
Num. H-bond donors : | 0.0 |
Molar Refractivity : | 11.75 |
TPSA : | 40.13 Ų |
GI absorption : | High |
BBB permeant : | Yes |
P-gp substrate : | No |
CYP1A2 inhibitor : | No |
CYP2C19 inhibitor : | No |
CYP2C9 inhibitor : | No |
CYP2D6 inhibitor : | No |
CYP3A4 inhibitor : | No |
Log Kp (skin permeation) : | -7.0 cm/s |
Log Po/w (iLOGP) : | 0.0 |
Log Po/w (XLOGP3) : | 0.91 |
Log Po/w (WLOGP) : | 0.56 |
Log Po/w (MLOGP) : | 0.27 |
Log Po/w (SILICOS-IT) : | 0.93 |
Consensus Log Po/w : | 0.53 |
Lipinski : | 0.0 |
Ghose : | None |
Veber : | 0.0 |
Egan : | 0.0 |
Muegge : | 1.0 |
Bioavailability Score : | 0.55 |
Log S (ESOL) : | -1.72 |
Solubility : | 4.24 mg/ml ; 0.0192 mol/l |
Class : | Very soluble |
Log S (Ali) : | -1.34 |
Solubility : | 10.1 mg/ml ; 0.0459 mol/l |
Class : | Very soluble |
Log S (SILICOS-IT) : | -0.08 |
Solubility : | 182.0 mg/ml ; 0.826 mol/l |
Class : | Soluble |
PAINS : | 0.0 alert |
Brenk : | 0.0 alert |
Leadlikeness : | 1.0 |
Synthetic accessibility : | 1.0 |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
2.3 g | Stage #1: With sodium carbonate In water at 20℃; for 0.5 h; |
2.5 g (0,0147 M) AgNO3was dissolved in20 cm3 of water in a 100 ml flask, then solution of1.715 g (0,0162 M) sodium carbonate in 30 cm3 ofwater was added drop wise slowly at room temperature to the AgNO3 solution, stirred for 30minutes, the precipitate was filtered off, washed withwater and dried in a vacuum-desiccator.Trifluoroacetic acid was poured to the residue andthe solution was stirred with a magnetic stirrer,rotary evaporated and dried under vacuum. Theyield is 2.3 g of silver trifluoroacetate. Found: C-10,859 percent, Obtained: C-11,105 percent. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
1.5 g | at 20℃; | 3.4 g of sodium trifluoroacetate was dissolved in 6 g of water to prepare an aqueous solution. An aqueous solution prepared by dissolving 3.39 g of silver nitrate in 3 g of water was added thereto at room temperature. The resulting aqueous solution was extracted 10 times with 5 ml of diethyl ether and the combined extracts were dried over anhydrous magnesium sulfate. The magnesium sulfate was filtered off and the ether solution was concentrated on a rotary evaporator to precipitate a white solid. Further, the mixture was dried by heating on a rotary evaporator under reduced pressure at 50 ° C. for 2 hours to obtain 1.5 g of a white powder of silver trifluoroacetate. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In water |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In dichloromethane; at 20℃; for 0.0833333h;Darkness; | Au(PPh3)Cl (99 mg, 0.2 mmol) was added to a solution of silver trifluoroacetate (44 mg, 0.2 mmol) in anhydrous CH2Cl2 (2 mL) in the dark. The reaction mixture was stirred for 5 min at r.t. and then allowed to stand for 5-10 min. The upper solution of Au(Ph3P)OTFA had a concentration of 0.1 mmol/mL in CH2Cl2 and was used directly. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
30% | With AgCN; AgBF4 In water excess Ag2C2 and AgCN added to concd. aq. soln. of AgCF3CO2 and AgBF4 (molar ratio ca. 1:1); stirred until satn.; filtered; (15)crown-5 added tofiltrate; placed in desiccator (P2O5); flame-sealed; kept at 115.degree .C (6 h); cooled to room temp.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
50% | With AgBF4 In water Ag2C2 added to concd. aq. soln. of AgCF3CO2 and AgBF4; stirred until satn.; excess Ag2C2 filtered off; (15)crown-5 added to filtrate; allowed tostand (several h); |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In not given |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
77% | In tetrahydrofuran; methanol Ag-salt in methanol was added to a soln. of Ph3PAuCl in THF, the mixt. was stirred for 30 min, filtered, a soln. of thiobarbituric acid in DMF was added, the mixt. was stirred for 1 h; filtered, washed with DMF, CH2Cl2, acetone, ether; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | In dichloromethane byproducts: AgCl; to soln. Au complex in CH2Cl2 CF3COOAg was added and stirred at room temp. for 30 min, suspn. was filtered through Celite, ligand mercaptobenzimidazole was added and stirred at room temp. overnight; soln. was concd., Et2O was added, ppt. was filtered and washed with Et2O, recrystn. from CH2Cl2 by diffusion Et2O - mixt. isomers; elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol; water equimol., a soln. of triazole compd. (etahnol) layered upon a soln. of Ag salt (water), 1 mn; XRD; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
66% | AgTFA (22mg, 0.1mmol) and dppe (20mg, 0.05mmol) were stirred in 6mL THF for an hour and then 4-PAH (15.0mg, 0.1mmol), neutralised in 4mL water by NaOH (aq.), was added dropwise. The mixture was stirred for another 1h before the white precipitate was filtered, washed and dried. The dried powder was dissolved in 8mL 1:1 mixture of water and acetonitrile. Diffraction quality single crystals were obtained by layering diethyl ether over it, Yield: 65%. 1H NMR (300MHz, d6-DMSO, 298K): deltaH=8.59 (d, Py-H), 7.74-7.67 (m, Ar-H, dppe), 7.61 (d, Py-H), 7.56-7.42 (m, Ar-H, dppe and CH=CH), 6.81 (d, CH=CH), ?2.6 (s, CH-CH, dppe). Anal. Calc. (without solvent): C, 55.54; H, 4.13; N, 4.42. Found: C, 55.44; H, 5.10; N, 3.75%. No solvent loss was observed in TGA experiment |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | AgTFA (22mg, 0.1mmol) and PPh3 (27mg, 0.1mmol) were stirred in 6mL THF for an hour. Then 4-PAH (15mg, 0.1mmol) neutralised with equivalent amount of NaOH (aq.) in 3mL water was added dropwise. White precipitate was formed and the mixture was continued stirring for another hour. White precipitate was filtered off and washed with water and THF. The dried precipitate was dissolved in 10mL 1:1 mixture of water and acetonitrile and then diethyl ether was layered over this solution. Diffraction quality single crystals were obtained after a few days. Yield: 70%. 1H NMR (300MHz, d6-DMSO, 298K): deltaH=8.54 (d, Py-H), 7.54-7.49 (m, Ar-H, PPh3 and Py-H), 7.24 (d, CH=CH), 6.77 (d, CH=CH). The observed solvent loss of 5.8% in TGA experiment was compared with calculated value, 5.9% for the composition C53H48.5Ag2N2.5O6.5P2 (excluding diethyl ether molecules and adding hydrogen atoms for water molecules to the formula unit). Anal. Calc. for C53H48.5Ag2N2.5O6.5P2: C, 57.76; H, 4.44; N, 3.18. Found: C, 57.70; H, 4.65; N 2.68%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | AgTFA (22mg, 0.1mmol) and <strong>[2071-20-7]dppm</strong> (38mg, 0.1mmol) were stirred in 6mL THF for an hour and then Hpvba (22mg, 0.1mmol) neutralised with equivalent amount of NaOH (aq.) in 4mL water was added dropwise. The mixture was stirred for another hour. The white precipitate was filtered, washed with water and THF and was then dried. The dried powder was dissolved in 8mL 1:1 mixture of water and CH3CN. Diffraction quality single crystals were grown by slowly evaporation. Yield: 78%. 1H NMR (300MHz, d6-DMSO, 298K): deltaH=8.60 (d, Py-H), 8.20 (d, Ar-H), 7.81 (d, Py-H), 7.41 (d, CH=CH), 7.66 (m, Ar-H, <strong>[2071-20-7]dppm</strong>), 7.27 (m, Ar-H, pvba, <strong>[2071-20-7]dppm</strong>) 7.12 (m, CH=CH, Ar-H, <strong>[2071-20-7]dppm</strong>), 3.85 (m, CH2, <strong>[2071-20-7]dppm</strong>). Anal. Calc. for C132H108Ag4F6N2O8P8: C, 59.97; H, 4.12; N, 1.06. Found: C, 59.91; H, 4.14; N, 1.49%. No solvent loss was observed in TGA experiment. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | In acetonitrile; for 0.5h; | General procedure: Pyridine-4-amidoxime (0.5mmol, 0.069g) was added to a stirred acetonitrile solution (20mL) of silver(I) perchlorate (0.5mmol, 0.101g). The reaction mixture was stirred for half an hour. The solution turned a pale yellow colour and was filtered. The filtrate was kept in dark for slow evaporation. Colorless rod shaped single crystals of 2 were obtained after 25days. Yield: 60%, 0.102g. Anal. Calc. for C6H7AgClN3O5: C, 20.92; H, 2.05; N, 12.20. Found: C, 20.87; H, 2.01; N, 12.23%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
87.9% | In acetonitrile for 0.25h; Inert atmosphere; Schlenk technique; | 2.2.7 Synthesis of (Agtfa)2(BPMP-3)(5,5′-dimethyl-2,2′-dipyridyl)2 (6) One equivalent of BPMP-3 (0.100 g, 0.198 mmol) in 5 mL of acetonitrile was added to a solution of one equivalent of Agtfa (0.0879 g, 0.398 mmol) in 5 mL of acetonitrile. A solution of 5,5′-dimethyl-2,2′-dipyridyl (0.0729 g, 0.396 mmol) in 5 mL of acetonitrile was added and stirred for 15 min. After drying in vacuo, 1 mL of acetonitrile was added to the crude product and 30 mL of diethyl ether was added to precipitate 6. The supernatant was removed via cannula and 6 was isolated as a white solid in an 87.9% yield (0.229 g, 0.174 mmol). Colorless block crystals of 6 were obtained from vapor diffusion of diethyl ether into a DMF solution at 5 °C. 1H NMR (360.13 MHz, CD3CN, 298 K): δ 8.28 (s, 4H, Hg), 8.26 (dd, JH,H=4.8Hz, 1.7Hz, 1H, Hc), 8.08 (d, JH,H=8.3Hz, 4H, He), 8.01 (s, 1H, Hd), 7.80 (d, JH,H=8.1Hz, 4H, Hf), 7.46 (m, 12H), 7.34 (m, 8H), 7.04 (d, JH,H=7.7Hz, 1H, Ha), 6.93 (dd, JH,H=7.6Hz, 4.8Hz, 1H, Hb), 4.06 (s, 4H, Ph2P-CH2-), 3.92 (s, 2H, N-CH2-), 2.30 (s, 12H, Hh). 31P{1H} NMR (145.78 MHz, CD3CN, 298 K): δ -5.9 (s). 31P{1H} NMR (202.33 MHz, CD3CN, 240 K): δ -9.3 (br s), -6.3 (br s). Anal. Calc. for Ag2P2N6C60H54O4F6·2H2O: C, 53.35; H, 4.33; N, 6.22. Found: C, 53.66; H, 4.17; N, 6.33%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
87.9% | In acetonitrile for 0.25h; Inert atmosphere; Schlenk technique; Darkness; | 2.2.2. Synthesis of [Ag(BPMP-3)2][BF4] (1) One equivalent of BPMP-3 (0.100 g, 0.198 mmol) in 5 mL of acetonitrile was added to a solution of one equivalent of Agtfa(0.0879 g, 0.398 mmol) in 5 mL of acetonitrile. A solution of 5,5'-dimethyl-2,2'-dipyridyl (0.0729 g, 0.396 mmol) in 5 mL of acetonitrile was added and stirred for 15 min. After drying in vacuo, 1 mL of acetonitrile was added to the crude product and 30 mL of diethyl ether was added to precipitate 6. The supernatant was removed via cannula and 6 was isolated as a white solid in an 87.9% yield (0.229 g, 0.174 mmol). Colorless block crystals of 6 were obtained from vapor diffusion of diethyl ether into a DMF solution at 5 °C. 1H NMR (360.13 MHz, CD3CN, 298 K): δ 8.28 (s,4H, Hg), 8.26 (dd, JH,H = 4.8 Hz, 1.7 Hz, 1H, Hc), 8.08 (d, JH,H = 8.3 Hz,4H, He), 8.01 (s, 1H, Hd), 7.80 (d, JH,H = 8.1 Hz, 4H, Hf), 7.46 (m, 12H),7.34 (m, 8H), 7.04 (d, JH,H = 7.7 Hz, 1H, Ha), 6.93 (dd, JH,H = 7.6 Hz,4.8 Hz, 1H, Hb), 4.06 (s, 4H, Ph2P-CH2-), 3.92 (s, 2H, N-CH2-),2.30 (s, 12H, Hh). 31P{1H} NMR (145.78 MHz, CD3CN, 298 K): δ 5.9 (s). 31P{1H} NMR (202.33 MHz, CD3CN, 240 K): δ 9.3 (br s),6.3 (br s). Anal. Calc. for Ag2P2N6C60H54O4F62·H2O: C, 53.35; H,4.33; N, 6.22. Found: C, 53.66; H, 4.17; N, 6.33%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75% | In dichloromethane for 0.25h; Inert atmosphere; Schlenk technique; Darkness; | 7 2.2.7 Synthesis of (Agtfa)2(DPAP-2)(5,5′-dimethyl-2,2′-dipyridyl)2 (6) One equivalent of DPAP-2 (0.100g, 0.334mmol) in 5mL of DCM was reacted with two equivalents of Agtfa (0.146g, 0.663mmol) in 5mL of DCM. To this mixture, two equivalents of 5,5′-dmbpy (0.122g, 0.662mmol) in 5mL of DCM was added. After the solution stirred for 15min, the solvent was removed under vacuum to yield crude product. The crude product was dissolved in 1mL of DCM, and 6 was precipitated by the addition of 30mL of diethyl ether. After the supernate was extracted, 6 was dried under vacuum and the off-white solid was isolated in a 75% yield (0.276g, 0.251mmol). Crystals were obtained by slow vapor diffusion of diethyl ether into a solution of THF containing 6 at 5°C. 1H NMR (400.13MHz, CD3OD, 300K): δ 8.32 (s, 4H, He), 8.05 (d, JH,H=8.2Hz, 4H, Hf/g), 7.79 (m, 8H), 7.55 (m, 7H), 7.20 (t, JH,H=7.2Hz, 1H, Hb), 6.83 (d, JH,H=8.5Hz, 1H, Ha), 6.57 (t, JH,H=6.1Hz, 1H, Hc), 6.21 (br s, 1H, N-H), 4.49 (d, JH,H=5.6Hz, 2H, -CH2-), 2.35 (s, 12H, Hh). 31P{1H} NMR (161.97MHz, CD3CN, 300K): δ 1.4 (s). Anal. Calc. for Ag2F6N6O4PC46H41·H2O (1102.57): C, 49.31; H, 3.87; N, 7.50. Found: C, 49.31; H, 3.84; N, 7.22%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
59.82% | In m-xylene; for 0.5h; | General procedure: Complex 1 was prepared by mixing of AgCF3COO (0.0142 g,0.0641 mmol) and p-phda (0.0050 g, 0.0317 mmol) in 2 mLbenzene. After stirring for 30 min, the resultant solution was introducedinto a 9 mm diameter glass tube and layered with n-pentane(2 mL) as a diffusion solvent. After standing at room temperaturefor one week, colorless crystals of 1 suitable for single crystal X-ray analysis were obtained. Yield (based on p-phda): 96.52%.Anal. Calc. for C19H11Ag3F9N2O6 C, 38.53; N, 2.06; H, 1.35. Found:C, 38.36; N, 2.12; H, 1.66%. IR (KBr, m/cm1): 3450(w), 2249(w),1680(s), 1518(w), 1423(m), 1209(s), 1130(s), 839(m), 804(m),723(s). 1H NMR (DMSO-d6, d/ppm): 7.380 (phenyl, p-phda), 7.369(CH, benzene), 4.053(CH2, p-phda). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96.52% | for 0.5h; | Complex 1 was prepared by mixing of AgCF3COO (0.0142 g,0.0641 mmol) and p-phda (0.0050 g, 0.0317 mmol) in 2 mLbenzene. After stirring for 30 min, the resultant solution was introducedinto a 9 mm diameter glass tube and layered with n-pentane(2 mL) as a diffusion solvent. After standing at room temperaturefor one week, colorless crystals of 1 suitable for single crystal X-ray analysis were obtained. Yield (based on p-phda): 96.52%.Anal. Calc. for C19H11Ag3F9N2O6 C, 38.53; N, 2.06; H, 1.35. Found:C, 38.36; N, 2.12; H, 1.66%. IR (KBr, m/cm1): 3450(w), 2249(w),1680(s), 1518(w), 1423(m), 1209(s), 1130(s), 839(m), 804(m),723(s). 1H NMR (DMSO-d6, d/ppm): 7.380 (phenyl, p-phda), 7.369(CH, benzene), 4.053(CH2, p-phda). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In dichloromethane; water; at 20℃; for 2h;Schlenk technique; | A solution of AgOCOCF3 (0.331 g, 1.51 mmol) dissolved in H2O (2 mL) was added to a Schlenk flask containing [PdCl2(TMEDA)] (0.200 g, 0.69 mmol) in CH2Cl2 (30 mL). After stirring the reaction mixture for 2 h at room temperature, white solids precipitated. The mixture was filtered to remove the salts and dried over CaCl2. The solvent was completely removed under vacuum. The resulting residue was solidified with hexane. The solids were washed with n-hexane (2 mL × 2) to give crude solids, which were recrystallized from CH2Cl2/hexane to give compound 1. The complex 1 was also prepared from [Pd(TFA)2] and TMEDA (N,N,N',N'-tetramethylethylenediamine)under reflux.9 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
77% | In ethanol at 20 - 60℃; for 0.166667h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
95% | In methanol at 20℃; for 1h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
61% | With 4,7-dimethoxy-1,10-phenanthroline; Selectfluor; cesium fluoride at 50℃; Inert atmosphere; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
63% | In methanol; acetone; at 20℃; for 3h;Darkness; | General procedure: Silver(I) complexes [Ag(NO3-O)(4,7-phen-mu-N4,N7)]n (1), [Ag(CF3COO-O)(4,7-phen-mu-N4,N7)]n (3) and [Ag2(H2O)(4,7-phen-mu-N4,N7)2](BF4)2}n (5) were synthesized according to the modified procedure for the preparation of silver(I) complexes with diazanaphthalenes [17]. A solution of 4,7-phen (36.0mg, 0.2mmol) in 10mL of warm acetone was added slowly with stirring to a solution containing 0.4mmol of the corresponding silver(I) salt (67.9mg of AgNO3 for 1, 88.4mg of AgCF3COO for 3 and 77.9mg of AgBF4 for 5) dissolved in 10mL of warm methanol. The reaction mixture was stirred in the dark at room temperature for 3h. The white precipitate that formed immediately on addition of 4,7-phen was filtered off and dissolved in the corresponding solvent (acetonitrile for 1, ethanol for 3 and methanol for 5). The obtained solution was left to evaporate slowly at room temperature. After 3-5days, colorless crystals of 1, 3 and 5, suitable for single crystal X-ray analysis were formed. Yield (calculated on the basis of N-heterocyclic ligand): 52.5mg (75%) for 1, 50.5mg (63%) for 3 and 69.8mg (87%) for 5. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
65% | In ethanol; at 25℃; for 3h;Darkness; | General procedure: Silver(I) complexes, [Ag(NO3)(<strong>[254-79-5]1,5-naph</strong>)]n (Ag1), [Ag(CF3COO)(<strong>[254-79-5]1,5-naph</strong>)]n (Ag2) and [Ag(CF3SO3)(<strong>[254-79-5]1,5-naph</strong>)]n (Ag3), were synthesized according to the modified procedure for the preparation of silver(I) complexes with phthalazine and quinazoline [29]. The solution of 1.0mmol of the corresponding silver(I) salt (169.9mg of AgNO3 for Ag1, 220.9mg of AgCF3COO for Ag2 and 256.9mg of AgCF3SO3 for Ag3) in 10mL of ethanol was added slowly under stirring to the solution containing an equimolar amount of <strong>[254-79-5]1,5-naph</strong> (130.2mg) in 5mL of ethanol. A white precipitate was formed after addition of the N-heterocyclic ligand. The reaction mixture was stirred in the dark at room temperature for 3h, and then, the precipitate was filtered off and recrystallized in methanol (Ag1) or ethanol (Ag2 and Ag3). The obtained solution was left at room temperature and after 3-5days, colorless crystals of Ag1-3 suitable for single-crystal X-ray analysis, were formed. Yield (calculated on the basis of the N-heterocyclic ligand): 216.0mg (72%) for Ag1, 228.2mg (65%) for Ag2 and 263.2mg (68%) for Ag3. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
88% | With dichloro(pentamethylcyclopentadienyl)rhodium (III) dimer; copper diacetate In ethanol at 80℃; for 0.5h; | |
88% | With dichloro(pentamethylcyclopentadienyl)rhodium (III) dimer; copper diacetate In ethanol at 80℃; for 0.5h; Inert atmosphere; | 2 The 1-phenyl-3,4-dihydroisoquinol 1a (104mg, 0.5mmol),1,-2-Diphenylacetylene 2a (89.1mg, 0.5mmol),Dichloro(pentamethylcyclopentadienyl) rhodium(III) dimer [(Cp*RhCl2)2, 1.05mg, 0.5%mmol],AgOOCCF3 (165.6 mg, 0.75 mmol) and Cu(OAc) 2 (90.8 mg, 0.5 mmol) were added to a 25 mL round bottom flask, and then 5 mL of absolute ethanol was added.The reaction was stopped after heating and refluxing for 30 minutes under the protection of N2.Filter with 100-200 mesh silica gel and wash with ethanol.After collecting the organic phase, the organic solvent was distilled off under reduced pressure, and the residue was separated and purified by 200-300 mesh silica gel column chromatography, eluted with dichloromethane/methanol=20:1 (V/V)Obtained 219 mg of pure trifluoroacetate dihydroisoquinol salt derivative 3aa.The product was a light brown solid with a yield of 88%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
75% | In ethanol; acetone; at 20℃; for 72h;Darkness; | Put 0.02g (0.1mmol) tert-butyl silver sulfide (ButSAg) in a mixed solution of 3mL acetone and 3mL ethanol, and quickly stir; add 0.02g (0.1mmol) silver trifluoroacetate (CF3COOAg) and stir until the solution is clear; Add 0.02 g (0.13 mmol) of <strong>[1571-33-1]phenylphosphonic acid</strong>, and finally add 0.02 g (0.12 mmol) of 4,4?-bipyridine (bpy), and continue stirring for 5 minutes. After the reaction, the solution was volatilized at room temperature in the dark for 3 daysAfter about 20mg light yellow massive crystals, the yield was 75%,After filtering, washing with ethanol, and drying at room temperature, an organic solvent-induced fluorescent color-changing material is obtained. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
94% | With dichloro(pentamethylcyclopentadienyl)rhodium (III) dimer; copper diacetate In ethanol at 80℃; for 0.5h; Inert atmosphere; | 17 The 6,7-dimethoxy 1-phenyl-3,4-dihydroisoquinol 1c (133.7mg, 0.5mmol),1-phenyl-1-hexyne 2b (79.1mg, 0.5mmol),Dichloro(pentamethylcyclopentadienyl) rhodium(III) dimer [(Cp*RhCl2)2, 1.05mg, 0.5%mmol], AgOOCCF3(165.6mg, 0.75mmol) and Cu(OAc)2 (90.8mg, 0.5mmol) was added to a 25mL round bottom flask,Then add 5 mL of absolute ethanol.The reaction was stopped after heating and refluxing for 30 minutes under the protection of N2, and filtered with 100-200 mesh silica gel and washed with ethanol.The organic phase was collected, and the organic solvent was distilled off under reduced pressure. The residue was separated and purified by 200-300 mesh silica gel column chromatography, and eluted with dichloromethane/methanol=20:1 (V/V) to obtain 252.7mg of pure trifluoroacetic acid. Acid salt dihydroisoquinol salt derivative 3bc.The product is yellow oily viscous liquid,The yield was 94%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | With dichloro(pentamethylcyclopentadienyl)rhodium (III) dimer; copper diacetate In ethanol at 80℃; for 0.5h; Inert atmosphere; | 18 The 6,7-dimethoxy 1-phenyl-3,4-dihydroisoquinol 1c (133.7mg, 0.5mmol),Dec-5-yne 2c (69.1mg, 0.5mmol),Dichloro(pentamethylcyclopentadienyl) rhodium(III) dimer [(Cp*RhCl2)2, 1.05mg, 0.5%mmol],AgOOCCF3 (165.6 mg, 0.75 mmol) and Cu(OAc) 2 (90.8 mg, 0.5 mmol) were added to a 25 mL round bottom flask, and then 5 mL of absolute ethanol was added.The reaction was stopped after heating and refluxing for 30 minutes under the protection of N2, and filtered with 100-200 mesh silica gel.Ethanol washing.The organic phase was collected, and the organic solvent was distilled off under reduced pressure. The residue was separated and purified by 200-300 mesh silica gel column chromatography, eluted with dichloromethane/methanol=20:1 (V/V)Obtain 220 mg of pure trifluoroacetate dihydroisoquinol salt derivative 3cc.The product is a yellow oily viscous liquid with a yield of 85%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
96% | With dichloro(pentamethylcyclopentadienyl)rhodium (III) dimer; copper diacetate In ethanol at 80℃; for 0.5h; Inert atmosphere; | 12 The 6-methoxy 1-phenyl-3,4-dihydroisoquinol 1b (118.7 mg, 0.5 mmol),1-phenyl-1-hexyne 2b (79.1mg, 0.5mmol),Dichloro(pentamethylcyclopentadienyl) rhodium(III) dimer [(Cp*RhCl2)2, 1.05mg, 0.5%mmol], AgOOCCF3(165.6mg, 0.75mmol) and Cu(OAc)2 (90.8mg, 0.5mmol) was added to a 25mL round bottom flask, and then 5mL of absolute ethanol was added.The reaction was stopped after heating and refluxing for 30 minutes under the protection of N2, and filtered with 100-200 mesh silica gel and washed with ethanol.The organic phase was collected, and the organic solvent was distilled off under reduced pressure. The residue was separated and purified by 200-300 mesh silica gel column chromatography, and eluted with dichloromethane/methanol=20:1 (V/V) to obtain 243.6mg of pure trifluoroacetic acid. Acid salt dihydroisoquinol salt derivative 3bb.The product is yellow oily viscous liquid,The yield was 96%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
97% | With dichloro(pentamethylcyclopentadienyl)rhodium (III) dimer; copper diacetate In ethanol at 80℃; for 0.5h; Inert atmosphere; | 13 The 6-methoxy 1-phenyl-3,4-dihydroisoquinol 1b (118.7 mg, 0.5 mmol),Dec-5-yne 2c (69.1mg, 0.5mmol),Dichloro(pentamethylcyclopentadienyl) rhodium(III) dimer [(Cp*RhCl2)2, 1.05mg, 0.5%mmol], AgOOCCF3(165.6mg, 0.75mmol) and Cu(OAc)2 (90.8mg, 0.5mmol) was added to a 25mL round bottom flask, and then 5mL of absolute ethanol was added.The reaction was stopped after heating and refluxing for 30 minutes under the protection of N2, and filtered with 100-200 mesh silica gel and washed with ethanol.The organic phase was collected, and the organic solvent was distilled off under reduced pressure. The residue was separated and purified by 200-300 mesh silica gel column chromatography, eluted with dichloromethane/methanol=20:1 (V/V)Obtained 236.5 mg of pure trifluoroacetate dihydroisoquinol salt derivative 3cb.The product is a yellow oily viscous liquid with a yield of 97%. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
67.7% | In N,N-dimethyl acetamide at 20℃; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
81% | In diethyl ether; dichloromethane at 20℃; for 0.75h; Darkness; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
91% | With oxygen In dichloromethane; ethyl acetate at 30℃; for 48h; | Synthesis of complex [(C1NNBiBTP)Co(DMAP)2][CF3COO] (5). Asolution of [(C1NNBiBTP)Co(DMAP)] (2) (0.741 g1.0 mmol) in dichloromethane (10 mL) was added to a solution of silver(I) trifluoroacetate (0.330 g, 1.5 mmol) and DMAP (0.122 g, 1.0 mmol) in10 mL of ethyl acetate, and the mixture was stirred at 30 C under an O2-atmosphere. After 48 h, the resultant mixture was filtered through Celite, and the volatile components of the filtrate were removed in vacuo. The final residue was recrystallized with dichloromethane and hexane, and the resulting precipitate was collected by filtration and dried under vacuum to give a brown solid. Yield 0.89 g (91%). 1H NMR (CDCl3, 400 MHz, ppm): δ 7.94-7.93 (Ar-H), 7.71-7.69 (Ar-H), 7.43-7.42 (Ar-H), 7.30 (Ar-H), 7.17-7.16 (Ar-H), 6.44-6.43 (Ar-H), 6.43(Ar-H), 5.18-5.17 (Ar-H), 3.99-3.95 (d, 2H, -NCH2), 3.77-3.74 (d, 2H,-NCH2), 3.24 (t, 2H, -NCH2), 2.96 (s, 6H, -NCH3), 2.68 (s, 6H, -NCH3), 2.32 (Ar-CH3), 2.00 (s, 2H, -NCH2), 1.21 (s, 6H, -NCH3). 13C NMR(CDCl3, 100 MHz, ppm): δ 154.62, 154.11, 152.53, 148.08, 146.14, 144.63, 134.07, 132.94, 126.35, 124.92, 121.57, 118.41, 108.39, 106.57 (Ph), 64.03 (-NCH2-), 63.23 (-NCH2-), 56.67 (-NCH2-), 49.77(-NCH3), 39.06 (-NCH3), 38.66 (-NCH3), 20.00 (Ar-CH3). Anal. Calc. for C48H52CoF3N12O4*CH2Cl2: N, 15.83; C, 55.42; H, 5.13. Found: N, 16.32;C, 55.83; H, 5.33. m/z (ESI-MS, CH2Cl2): 863.0 ([M-CF3COO]+, calcd 863.37). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
72% | With oxygen In dichloromethane; ethyl acetate at 30℃; for 48h; | Synthesis of complex [(C1NNBiBTP)Co(tBuPy)2][CF3COO] (7). A solution of [(C1NNBiBTP)Co(tBuPy)] (2) (0.754 g1.0 mmol) in dichloromethane (10 mL) was added to a solution of silver(I) trifluoroacetate (0.330 g, 1.5 mmol) and tBuPy (0.15 mL, 1.0 mmol) in 10mL of ethyl acetate, and the mixture was stirred at 30 C under an O2-atmosphere. After 48 h, the resultant mixture was filtered through Celite, and the volatile components of the filtrate were removed in vacuo. The final residue was recrystallized with dichloromethane and hexane, and the resulting precipitate was collected by filtration and dried under vacuum to give a brown solid. Yield 0.72 g (72%). Anal. Calc. for C52H58CoF3N10O4*CH2Cl2: N, 12.87; C, 58.51; H, 5.56. Found:N, 12.80; C, 58.98; H, 5.31. m/z (ESI-MS, CH2Cl2) : 888.8 ([MCF3COO]+,calcd 889.41). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
90% | for 1h;Heating; | Compound 2 (0.585 g, yield 90%) has been prepared following aprocedure similar to that reported for 1 by using an acetonitrile solution(5 mL) of AgOOCCF3 (0.221 g, 1.0 mmol) and Pmes3 (0.388 g, 1.0mmol). M.p. 223-225 C. Anal. Calc. for C31H36AgF3O2NP: C, 57.24; H,5.58; N, 2.15%. Found: C, 57.20; H, 5.48; N, 2.03%. Λm (CH3CN, 10 4M): 121 Ω 1 cm2 mol 1. Λm (CH2Cl2, 10 4 M): 26 Ω 1 cm2 mol 1. IR(KBr, cm 1): 2303m, 2268s υ(CH3C- - -N), 1671vs, 1602s υ(CF3COO),1588m, 1550m υ(CC). IR (nujol, cm 1): 595m, 569s, 556s, 539w,518w, 512w, 459w, 426vs υ(Pmes3). 1H NMR (CDCl3, 293 K): δ, 1.82br,2.28s, 2.54br (30H, CH3CN and P(C6H2-2,4,6-(CH3)3)3), 6.87br (6H, P(C6H2-2,4,6-(CH3)3)3). 19F NMR (CDCl3, 223 K): δ, 74.1s. 31P NMR(CDCl3, 293 K): δ, 29.9dd (1J(31P-109Ag): 804.8 Hz; 1J(31P-107Ag):697.4 Hz). 31P NMR (CDCl3, 223 K): δ, 30.4dd (1J(31P-109Ag): 809.2Hz; 1J(31P-107Ag): 699.4 Hz). |
Tags: 2966-50-9 synthesis path| 2966-50-9 SDS| 2966-50-9 COA| 2966-50-9 purity| 2966-50-9 application| 2966-50-9 NMR| 2966-50-9 COA| 2966-50-9 structure
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