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CAS No. :14040-11-0 MDL No. :MFCD00011462
Formula : C6O6W Boiling Point : -
Linear Structure Formula :- InChI Key :-
M.W : 351.90 Pubchem ID :-
Synonyms :

Safety of [ 14040-11-0 ]

Signal Word:Danger Class:6.1
Precautionary Statements:P261-P264-P270-P271-P280-P301+P310-P302+P352-P304+P340-P311-P330-P361-P363-P403+P233-P405-P501 UN#:3466
Hazard Statements:H301+H311+H331 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 14040-11-0 ]

* 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 [ 14040-11-0 ]

[ 14040-11-0 ] Synthesis Path-Downstream   1~96

  • 1
  • [ 14040-11-0 ]
  • [ 2071-20-7 ]
  • [ 41830-14-2 ]
YieldReaction ConditionsOperation in experiment
91% With sodium tetrahydroborate; at 120℃; under 760.051 Torr; for 0.666667h;Microwave irradiation; Inert atmosphere; Green chemistry; General procedure: The reactions were run in a CEM Corp. MARS microwave fitted with a fiber optic temperature probe and a port on top for a reflux condenser.1 mmol of Mo(CO)6 and dppe (0.425 g, 1.1 mmol) were combined with 20 mL of 1-propanol in a two-neck 100 mL RB flask. To this mixture was added NaBH4 (0.128 g, 3.3 mmol). The flaskwas placed in themicrowave and a reflux condenser attached through a hole in the top of the microwave. The mixture was sparged with nitrogen. The mixture was heated under nitrogen at 400 W for 1.5 min to reach reflux temperature. Once the reflux temperature was reached the microwave power was reduced and the temperature maintained for 18 min. The mixture was cooled to room temperature and 2-4 mL of water was added to the reaction to dissolve excess NaBH4 and promote product precipitation. The reaction was cooled -10 C for several hours. The light yellow complex was filtered in air and washed with 2×5 mL of petroleum ether/diethyl ether(1:1) mixture resulting in 580 mg of Mo(CO)4dppe after drying, a 95% yield.
  • 2
  • [ 109-99-9 ]
  • [ 14040-11-0 ]
  • [ 36477-75-5 ]
YieldReaction ConditionsOperation in experiment
at 20℃; for 3h;Photolysis; UV-irradiation; Inert atmosphere; Schlenk technique; A solution of W(CO)5·THF (0.62 mmol), prepared by photolysis of W(CO)6 (0.22 g, 0.62 mmol) in THF (20 ml), using a low-pressure mercury immersion lamp in a quartz flask during 3 h at room temperature, was added to a solution of BnN(CH2CH2NC6F5)2Ge (1) (0.37 g, 0.62 mmol) in THF (10 ml). The reaction mixture was stirred for 2 days at room temperature in the dark and the volatiles were removed under vacuum. Then ether (10 ml) was added to the residue, the precipitate was filtered off to give 6 (0.14 g, 73%) as a white solid. 1H NMR (400 MHz, C6D6): δ = 1.95-2.05, 2.81-2.90 (2m, 4H, 2CH2N), 3.16-3.23, 3.25-3.30 (2m, 4H, 2CH2NC6F5), 4.19 (s, 2H, CH2Ph), 6.73-6.76, 6.96-7.10 (2m, 5H, Ph) ppm. 13C NMR (100 MHz, C6D6): δ = 53.36 (СH2N), 56.38 (CH2NC6F5), 64.02 (CH2Ph), 129.16, 129.89, 129.98, 130.86 (Ph), 196.57 (1JW-C = 122 Hz, cis-СО), 198.33 (1JW-C = 150 Hz, trans-СО) ppm. The 13C NMR signals of the pentafluorophenyl rings were not observed under these conditions due to poor solubility and high order C-F coupling. 19F NMR (376.4 MHz, C6D6): δ = -148.50 to -148.70 (m, 2F), -163.89 to -164.10 (m, 3F) ppm. IR (Nujol, cm-1): ν(C=O) 2056, 1986, 1945. C28H15F10GeN3O5W (919.8987): calcd. С 36.56, H 1.64, N 4.57; found C 36.62, H 1.77, N 4.59.
for 8h;Inert atmosphere; Irradiation; Compound 1 (0.10g, 0.2mmol) was added to a solution of W(CO)5THF in THF, prepared in situ by the irradiation of a solution of W(CO)6 (70mg, 0.2mmol) in THF (15ml) for 8h. The reaction mixture was stirred and heated at 45C for 4h. The solvent was removed under a reduced pressure, and the residue was purified by column chromatography on silica using ethyl acetate as the eluent. The eluate was concentrated to dryness, and the residue was recrystallized from CH2Cl2/hexane to give yellow crystals of 2. Yield: 43mg (26%). 1H NMR (DMSO-d6): δ 2.83 (s, 3H, CH3), 3.17 (s, 3H, CH3), 6.22 (s, 1H, CH), 7.29 (d, J=1.2 Hz, 1H), 7.38 (J=1.2Hz, 1H), 7.39 (J=1.3Hz, 1H), 7.57 (d, J=1.3Hz, 1H) (protons of imidazole), 7.42-7.50 (m, 6H), 7.69-7.91 (m, 4H) (C6H5) ppm. 13C NMR (DMSO-d6): δ 33.2, 33.3 (CH3), 36.2 (CH), 123.7, 125.5, 127.7, 128.7, 129.9, 134.3, 135.3, 142.5, 145.8, 146.6 (carbons of C6H5 and imidazole), 197.8 (4C), 201.8 (CO) ppm. 119Sn NMR (DMSO-d6): δ-234.0ppm. IR: νCO=2069.6 (m), 1977.0 (s), 1940.4 (vs), 1913.4 (vs), 1861.3 (vs) cm-1. Anal. Calc. for C26H21ClN4O5SSnW: C, 37.20; H, 2.52; N, 6.67. Found: C, 37.46; H, 2.32; N, 6.37%.
Irradiation; Pentacarbonyl-η1P-(1-methyl-1H-1,3-benzazaphosphole-2-carboxylic acid)tungsten(0) (12a) A solution of W(THF)(CO)5 was prepared by irradiation of W(CO)6 (81 mg, 0.23 mmol), dissolved in THF (85 mL), by using a medium pressure mercury UV-immersion lamp (2.5 h, 20 C). Then 11a (40.6 mg, 0.21 mmol) was added. After stirring for 24 h the solvent was removed and the residue extracted with diethyl ether. Removal of the solvent gave 74 mg (68%) pale brown solid. 1H NMR (d8-THF): δ = 4.32 (d, 4JPH = 3.4 Hz, 3H, NCH3), 7.34 (tdd, 3J = 8.1, 6.9, 4J = 0.9, 5JPH = 2.1 Hz, 1H, H-5), 7.61 (ddt, 3J = 8.7, 6.9, 4J = 1.5, 5JPH = 2 Hz, 1H, H-6), 7.89 (br d, 3J = 8.7 Hz, 1H, H-7), 8.02 (tt, 3J ≈ 3JPH ≈ 8.1, 4J ≈ 5J ≈ 0.9 Hz, 1H, H-4). 13C{1H} NMR (d8-THF): δ = 35.38 (s, N-CH3), 115.63 (d, 3J = 4.0 Hz, C-7), 122.53 (d, 3J = 15.9 Hz, C-5), 128.36 (d, 4J = 11.9 Hz, C-6), 129.41 (d, 2J = 5.3 Hz, C-4), 137.89 (d, 1J = 25.3 Hz, Cq-3a), 146.37 (d, 2J = 2.7 Hz, Cq-7a), 154.21 (d, 1J = 27.9 Hz, COOH), 163.45 (d, 2J = 17.2 Hz, COOH), 195.29 (d, sat, 2J = 10.7, 1JCW = 126.0 Hz, 4 cis-CO), 200.15 (d, 2J = 33.2 Hz, trans-CO). 31P{1H} NMR (d8-THF): δ = 84.64 (satellites, 1JPW = 260.8 Hz). IR (KBr): νCO = 2078 (wm), 1928 (vs) cm-1. MS (EI, 70 eV, 90 C): m/z (%) = 517 (0.3) [M+], 461 (0.5), 377 (1.2), 349 (0.6), 306 (0.8), 193 (4.8). HRMS (ESI in MeOH): C14H9NO7PW (518.04), calcd. for [M(184W)+H]+ 517.9621; found: 517.9623 and correct isotopic pattern.
for 2.5h;Irradiation; Inert atmosphere; W(CO)6 (352 mg, 1.0 mmol) was dissolved in degassed THF (75 mL). The solution was irradiated with a medium pressure mercury vapor lamp under a slight N2 positive pressure for 2.5 h. The yellow solution of W(CO)5THF was transferred via cannula to a schlenk tube charged with 0.6 mmol of pyrimidine derivative. The solution was stirred 2 h at rt under N2 atmosphere. Concentration of the solvent under vacuum afforded a red solid which was crystallized from CH2Cl2/n-heptane.
at 20℃;UV-irradiation; Solid 1c·MeOH (170mg, 0.49mmol) was added to a solution of W(CO)5THF, prepared from W(CO)6 (380mg, 0.85mmol) in THF (60mL) at 20C by UV irradiation with a cooled mercury-immersion lamp (evolution of 19mL, 0.85mmol of CO). After stirring for 6h at room temperature the major part of the solvent was evaporated in vacuum. CH2Cl2 (15mL) was added to the residual 3-5mL, the mixture filtered and the solution stored for 3d at -24C. The pale yellow crystals (251mg) formed were separated, washed with CH2Cl2 (5mL) and dried in vacuum.
for 0.166667h;UV-irradiation; Inert atmosphere; Schlenk technique; General procedure: A THF solution of W(CO)6 (135 mg, 0.2 mmol) was irradiated with UV light under continuous stirring and argon atmosphere condition for 10 min. The colour of the solution changes from colourless to pale yellow. To the yellow reaction mixture dichloromethane solution of 7 (62 mg, 0.05 mmol) was added and subjected to room temperature stirring under inert atmosphere for 30 min. The reaction was continuously monitored by TLC. After the completion of the reaction the solution was subjected to chromatographic work-up using preparative TLC with acetone/hexane (10:90 v/v) solvent mixture. The compounds obtained were red colored [Fe3Te2(CO)9(η2-dppf)W(CO)5] (13) and black, [Fe3Te2(CO)8(η2-dppf)W(CO)5] (14). Trace amount of unreacted 7 and some amount of decomposition were also observed.
at 50℃; for 1h;Inert atmosphere; Irradiation; W(CO)5·(thf)] was prepared by irradiation of <strong>[14040-11-0]tungsten hexacarbonyl</strong> (0.70 g, 2.0 mmol) in THF (20 mL) with a medium pressure mercury lamp (400 W). After irradiation for 1 h at 50 C, compound 1 (87 mg, 0.10 mmol) was added to the solution. After stirring of the mixture for 6 h at 50 C, the reaction mixture was filtered through a pad of Celite. The filtrate was evaporated to dryness under reduced pressure and the obtained residue was purified by column chromatography on silica gel (hexane). Recrystallization of the resulting solid from CH2Cl2/EtOH afforded complex 4a (78 mg, 66 μmol, 66%).
for 8h;Inert atmosphere; Irradiation; Compound 4 (0.23 g, 0.60 mmol) was added to a solution of W(CO)5THF in THF, prepared in situ by the irradiation of a solution of W(CO)6 (0.21 g, 0.60 mmol) in THF (40 ml) for 8 h, and the mixture was stirred and heated at reflux for 6 h. The solvent was removed in vacuo, and the residue was purified by column chromatography on silica using CH2Cl2/hexane (1:2, v/v) as the eluent. The yellow eluate was concentrated to dryness in vacuo to give a yellow solid of complex 6, which was recrystallized from CH2Cl2/hexane to afford yellow crystals. Yield: 90 mg (22%). 1H NMR: δ 2.37(s, 3H), 2.58 (s, 3H) (CH3), 6.29 (s, br, 2H, CH and H4 of pyrazole),7.04e7.39 (m, 12H, C6H5 and NH) ppm. When D2O was added, theintegrated peak areas at 6.29 and 7.04e7.39 ppm corresponded to1H and 10H, respectively. 13C NMR: δ 12.1, 19.2 (CH3), 76.9 (CH),109.4 (C4 of pyrazole), 120.6, 123.7,129.5,129.9, 146.2, 157.1 (C6H5 aswell as C3 and C5 of pyrazole), 197.2, 198.0, 198.9, 201.3 (CO and CS)ppm. IR: νNH 3171.1 (m); nC≡O 2006.2 (vs), 1884.6 (vs), 1837.9(vs) cm-1. Anal. Calc. for C24H20N4O4S2W: C, 42.62; H, 2.98; N, 8.28.Found: C, 42.82; H, 3.06; N, 8.09%.
for 8h;Irradiation; Inert atmosphere; Compound 1 (93 mg, 0.1 mmol) was added to a solution ofW(CO)5(THF) in THF, prepared in situ by the irradiation of asolution of W(CO)6 (35 mg, 0.1 mmol) in THF (20 mL) for 8 h, and the mixture was stirred and heated at reflux for 10 h. After the reaction was completed, the solvent was removedunder reduced pressure, and the residue was purified bycolumn chromatography on silica using CH2Cl2/hexane (1/1v/v) as eluent to give (Ph3Sn)2C(3,5-Me2Pz)(BtW(CO)5) (3)as a yellow solid.
at 20℃; for 7h;UV-irradiation; Schlenk technique; Inert atmosphere; General procedure: A solution of [W(CO)6] (0.365 g, 1.04 mmol) in 280 ml THF was irradiated with an UV-lamp for 7 h at ambient temperature. The yellow solution was slowly added to a suspension of bis(2-methoxyphenylmethanolate)tin(II) (1) (0.410 g, 1.04 mmol) in 20 ml THF and the suspension was left to stir overnight. The reaction mixture was concentrated at reduced pressure until a volume of 50 ml was obtained. Crystallization from reaction solution by gas phase diffusion of n-pentane gave compound 3 as pale yellow microcrystals. Yield: 0.245 g (54%); decomp. 130C. 1H NMR (CDCl3, 500.3MHz, TMS) δ [ppm] 3.80 (s, 3H, CH3O), 5.02 (s, 2H, CH2), 6.66 (d, 1H, 3JH,H=8.1Hz), 6.85 (t, 1H, 3JH,H=7.4Hz), 7.20 (m, 2H). 13C{1H} NMR (125.81MHz, CDCl3, TMS) δ [ppm] 54.3 (OCH3), 65.1 (CH2), 110.4, 121.4, 126.7, 130.9, 131.0, 157.3, 196.5 (eq. CO, 1J(183W-13C)=124Hz), 198.3 (ax. CO). 119Sn{1H} NMR (CDCl3, 111.9MHz, SnMe4) δ [ppm]-403 [2Sn, 2J(119Sn-117Sn)=144Hz], -164 [4SnW, 2J(119Sn-117Sn)=144Hz; 1J(119Sn-183W)=1578Hz], (as a result of hydrolysis, other minor signals also occurred with main signals at-347 [0.08: 1 (SnW), 2J(119Sn-117Sn)=114Hz] and-205 [(0.16: 1 (SnW), 2J(119Sn-117Sn)=114Hz]. 13C{1H} CP MAS NMR (100.62MHz) δ [ppm] 54.1 (br, CH3O), 64.9 (br, CH2), 110.7 (br), 122.1 (br), 127.4 (br), 130.7 (br, double intensity), 157.7 (br), 196.1 br, CO).
for 3 - 4h;Irradiation; W(CO)6(0.550 g, 1.56 mmol) was dissolved in 50mL dry tetrahydrofuran(Pharmco) and degassed in a round-bottom flask. The resulting solution was illuminated with a 100-W mercury arc lamp until nearly complete conversion to W(CO)5(THF) had been effected[26] as determined by infrared spectroscopy; this normally required 3 to 4 h of constant illumination.
at -70℃; for 1h;Inert atmosphere; UV-irradiation; A solution of W(CO)6 (0.306 g, 0.870 mmol) in THF (40 mL) was cooled to -70C and UV-irradiated with argon bubbling. In 1 h, a yellow solution was formed.
In tetrahydrofuran; at 5℃; for 3h;UV-irradiation; Inert atmosphere; Synthesis of (1-isopropyl-2,3,4,5-tetraphenylphosphole)tungstenpentacarbonyl (2a) (general procedure). A solution of 0.35 g(1 mmol) of <strong>[14040-11-0]tungsten hexacarbonyl</strong> in tetrahydrofuran (100 mL)was irradiated with UV light in a quartz reactor for 3 h at 5 under continuous fl ow of argon. A solution of 1-isopropyl-2,3,4,5-tetraphenylphosphole (1a) (0.42 g, 1 mmol) in tetrahydrofuran(10 mL) was added to the resulting lemon-yellowsolution and the mixture was stirred for 12 h. The solvent wasevaporated in vacuo, the residue was extracted with n-hexane(40 mL) and fi ltered. The hexane extract was concentrated underreduced pressure, the residue was dried in vacuo to obtain 2a asa red powder The yield was 0.67 g (89%), m.p. 134 . 31P NMR(CDCl3), δ: 45.4 (s, 1JP,W = 215.9 Hz). 1H NMR (CDCl3), δ:1.26 (dd, 6 H, 3, 3JP, = 7.2 Hz, 3JH, = 15.9 Hz); 2.71-2.81(m, 1 H, ); 6.81-7.57 (m, 2 H, Ph); 7.01-7.32 (m, 14 H,Ph); 7.46-7.65 (m, 2 H, Ph); 7.80-7.87 (m, 2 H, Ph). 13C NMR(CDCl3), δ: 20.2 (s, CH3); 28.2 (d, , 1JC,P = 23.1 Hz); 126.7(s, p-CPh); 127.4 (s, p-CPh); 127.9 (s, m-CPh); 128.3 (s, m-CPh);129.6 (s, -CPh); 130.5 (s, -CPh); 131.6 (s, ipso-CPh); 137.9(s, ipso-CPh); 145.1 (s, C(3)/C(4)); 151.4 (d, C(2)/C(5),1JC,P = 17.2 Hz). IR (KBr), (CO)/cm-1: 1937, 2019, 2070,2128. Found (%): C, 57.64; H, 3.93; P, 4.17. C36H27O5PW(M 619). Calculated (%): C, 57.31; H, 3.61; O, 10.60; P, 4.11;W, 24.37.
for 1h;UV-irradiation; Inert atmosphere; Schlenk technique; Glovebox; W(CO)6 (43 mg, 0.13 mmol) is dissolved in 50 mL thf and irradiated with UV light for1 h using a low-pressure mercury lamp (TQ 150). The pale-yellow solution is added to asolution of [Cp”2Zr(1:1-As4)] (1) (50 mg, 0.067 mmol) and stirred for 24 h. After removingthe solvent in vacuo, the brown residue is extracted with n-hexane. Red crystals of 2suitable for single crystal X-ray structure analysis were obtained by storing a concentratedsolution at 78 C. Crystalline yield: 19 mg (0.014 mmol, 21%).1H NMR (C6D6, 298 K): d [ppm] = 1.26 (s, 36 H, CCH3), 5.31 (t, br, 2 H, C5H3tBu2),5.48 (d, 4 H, C5H3tBu2); IR (toluene): [cm1] = 2064 (m), 1977 (vs), 1937 (s); elementalanalysis (%): calculated for [C36H42ZrAs4W2O10] (1391.77 g/mol): C, 31.03; H, 3.04; O,11.48. No satisfying elemental analysis could be obtained, not even by using Sn capsules.This is caused by the air sensitivity of compound 2; FD MS (toluene): m/z (%): 1393.8(12) [M]+, 1070.2 (M+-[W(CO)5], 100); crystal data for C36H42As4O10W2Zr, triclinic, P-1, a = 11.0989(3) Å, b = 12.5065(3) Å, c = 17.5582(5) Å, = 101.764(2), = 95.394(2), = 113.207(2), V = 2151.41(10) Å3.
UV-irradiation; Inert atmosphere; W(CO)5(THF)adduct, which was synthesized by the UV irradiation of a solution of W(CO)6 in THF
at 0℃; for 0.5h;UV-irradiation; Schlenk technique; Inert atmosphere; General procedure: A colorless solution of [M(CO) 5 (THF)]; (M = Cr, Mo, W) was prepared by UV photolysis of [M(CO) 6 ] in THF at 0 C for 30 minutes under nitrogen atmosphere [31a] . After the addition of phenylethynyl ferrocenyl telluride (52 mg, 0.13 mmol), the re- action mixture immediately turned into deep red (1:1 ratio, ligand:M(CO) 6 ) yielding, 2 (M = Cr, 52% yield), 3 (M = Mo, 60% yield) and 4 (M = W, 66% yield) or into deep violet for double co- ordinated complexes (1:2 ratio, ligand: [M(CO) 6 ]), 5 (M = Cr, 65% yield, 6 (M = Mo, 72% yield) and 7 (M = W, 78% yield).

Reference: [1]Chemische Berichte,1983,vol. 116,p. 230 - 237
[2]European Journal of Inorganic Chemistry,2005,p. 496 - 503
[3]Journal of the Chemical Society, Dalton Transactions,1999,p. 3893 - 3898
[4]Journal of Organometallic Chemistry,1995,vol. 485,p. 123 - 126
[5]Phosphorus, Sulfur and Silicon and the Related Elements,1997,vol. 131,p. 25 - 35
[6]Journal of the American Chemical Society,2002,vol. 124,p. 526 - 527
[7]Journal of the American Chemical Society,2002,vol. 124,p. 5260 - 5261
[8]Organometallics,1989,vol. 8,p. 955 - 960
[9]Organometallics,1989,vol. 8,p. 1030 - 1039
[10]Journal of the American Chemical Society,1989,vol. 111,p. 7094 - 7103
[11]European Journal of Inorganic Chemistry,2011,p. 3632 - 3643
[12]Organometallics,2000,vol. 19,p. 5787 - 5790
[13]European Journal of Inorganic Chemistry,2001,p. 725 - 732
[14]Journal of the Chemical Society, Dalton Transactions,1999,p. 2627 - 2632
[15]Zeitschrift fur Anorganische und Allgemeine Chemie,2001,vol. 627,p. 1855 - 1858
[16]European Journal of Inorganic Chemistry,2001,p. 2655 - 2659
[17]Zeitschrift fur Naturforschung, B: Chemical Sciences,2001,vol. 56,p. 1328 - 1339
[18]European Journal of Inorganic Chemistry,1999,p. 1813 - 1820
[19]Journal of Organometallic Chemistry,2002,vol. 656,p. 102 - 107
[20]Journal of the Chemical Society, Dalton Transactions,2002,p. 3280 - 3289
[21]Journal of the Chemical Society, Dalton Transactions,1996,p. 2173 - 2176
[22]Zeitschrift fur Anorganische und Allgemeine Chemie,2003,vol. 629,p. 1316 - 1321
[23]Organic and Biomolecular Chemistry,2003,vol. 1,p. 3054 - 3058
[24]Zeitschrift fur Anorganische und Allgemeine Chemie,
    Zeitschrift fuer Anorganische und Allgemeine Chemie,2003,vol. 629,p. 1936 - 1942
[25]European Journal of Inorganic Chemistry,2004,p. 2062 - 2065
[26]Journal of Organometallic Chemistry,2004,vol. 689,p. 2324 - 2337
[27]Dalton Transactions,2012,vol. 41,p. 143 - 148
[28]Zeitschrift fur Anorganische und Allgemeine Chemie,2004,vol. 630,p. 2438 - 2449
[29]Dalton Transactions,2004,p. 3575 - 3585
[30]New Journal of Chemistry,2005,vol. 29,p. 154 - 164
[31]Dalton Transactions,2006,vol. 6,p. 1424 - 1433
[32]Zeitschrift fur Anorganische und Allgemeine Chemie,2006,vol. 632,p. 588 - 592
[33]Journal of Organometallic Chemistry,2006,vol. 691,p. 2734 - 2738
[34]Zeitschrift fur Naturforschung, B: Chemical Sciences,2006,vol. 61,p. 820 - 824
[35]Inorganic Chemistry,2007,vol. 46,p. 179 - 185
[36]Journal of Organometallic Chemistry,2006,vol. 691,p. 4963 - 4967
[37]Dalton Transactions,2008,p. 1831 - 1842
[38]Journal of the American Chemical Society,2009,vol. 131,p. 16233 - 16243
[39]Journal of Organometallic Chemistry,2012,vol. 713,p. 80 - 88
[40]Dalton Transactions,2013,vol. 42,p. 1144 - 1158
[41]Asian Journal of Chemistry,2013,vol. 25,p. 3113 - 3116
[42]Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry,2013,vol. 43,p. 305 - 311
[43]Journal of Organometallic Chemistry,2013,vol. 735,p. 15 - 25
[44]Inorganic Chemistry,2013,vol. 52,p. 11438 - 11449
[45]RSC Advances,2014,vol. 4,p. 6878 - 6885
[46]Journal of Polymer Science, Part A: Polymer Chemistry,2014,vol. 52,p. 664 - 670
[47]Journal of Organometallic Chemistry,2014,vol. 757,p. 8 - 13
[48]Organometallics,2014,vol. 33,p. 804 - 816
[49]Journal of Organometallic Chemistry,2014,vol. 758,p. 55 - 59
[50]Russian Journal of Coordination Chemistry,2010,vol. 36,p. 891 - 896
    Koord. Khim.,2010,vol. 36,p. 903 - 908,6
[51]Journal of Organometallic Chemistry,2014,vol. 763-764,p. 44 - 51
[52]Heteroatom Chemistry,2013,vol. 24,p. 452 - 459
[53]Chemistry - A European Journal,2014,vol. 20,p. 5708 - 5720
[54]Dyes and Pigments,2015,vol. 113,p. 562 - 570
[55]Tetrahedron,2015,vol. 71,p. 4933 - 4945
[56]Journal of Organometallic Chemistry,2015,vol. 794,p. 88 - 95
[57]Organometallics,2015,vol. 34,p. 4293 - 4304
[58]Chemistry Letters,2015,vol. 44,p. 1240 - 1242
[59]European Journal of Inorganic Chemistry,2015,vol. 2015,p. 4996 - 5002
[60]Dalton Transactions,2015,vol. 44,p. 16728 - 16736
[61]Chinese Journal of Chemistry,2015,vol. 33,p. 739 - 748
[62]Chemical Communications,2016,vol. 52,p. 613 - 616
[63]Organometallics,2015,vol. 34,p. 5703 - 5708
[64]Dalton Transactions,2016,vol. 45,p. 2261 - 2272
[65]Chemical Communications,2015,vol. 51,p. 11272 - 11275
[66]Angewandte Chemie - International Edition,2015,vol. 54,p. 15060 - 15063
    Angew. Chem.,2015,vol. 127,p. 15274 - 15277,4
[67]European Journal of Inorganic Chemistry,2016,vol. 2016,p. 691 - 699
[68]Dalton Transactions,2016,vol. 45,p. 2172 - 2179
[69]Dalton Transactions,2016,vol. 45,p. 2208 - 2217
[70]Dalton Transactions,2016,vol. 45,p. 2218 - 2226
[71]Dalton Transactions,2016,vol. 45,p. 2859 - 2867
[72]Journal of Organometallic Chemistry,2016,vol. 819,p. 53 - 60
[73]Transition Metal Chemistry,2016,vol. 41,p. 655 - 661
[74]Journal of Organometallic Chemistry,2016,vol. 821,p. 206 - 213
[75]Dalton Transactions,2017,vol. 46,p. 3556 - 3568
[76]Chemistry - A European Journal,2017,vol. 23,p. 10319 - 10327
[77]Inorganic Chemistry,2017,vol. 56,p. 10061 - 10069
[78]Dalton Transactions,2017,vol. 46,p. 7791 - 7799
[79]Australian Journal of Chemistry,2017,vol. 70,p. 1006 - 1015
[80]Dalton Transactions,2017,vol. 46,p. 15317 - 15329
[81]European Journal of Inorganic Chemistry,2017,vol. 2017,p. 4627 - 4634
[82]Russian Journal of Coordination Chemistry,2017,vol. 43,p. 837 - 842
    Koord. Khim.,2017,vol. 43,p. 739 - 743,5
[83]Angewandte Chemie - International Edition,2017,vol. 56,p. 15886 - 15890
    Angew. Chem.,2017,vol. 129,p. 16102 - 16106,5
[84]Russian Journal of Coordination Chemistry,2018,vol. 44,p. 647 - 652
[85]Journal of Organometallic Chemistry,2019,vol. 880,p. 341 - 348
[86]Chemistry - A European Journal,2019,vol. 25,p. 2262 - 2271
[87]Chemistry - A European Journal,2019,vol. 25,p. 4793 - 4807
[88]Dalton Transactions,2019,vol. 48,p. 2399 - 2406
[89]Organometallics,2019,vol. 38,p. 2403 - 2407
[90]Inorganic Chemistry,2019,vol. 58,p. 14931 - 14937
[91]Angewandte Chemie - International Edition,2019,vol. 58,p. 16092 - 16096
    Angew. Chem.,2019,vol. 131,p. 16238 - 16242,5
[92]Chemistry - A European Journal,2020,vol. 26,p. 1518 - 1524
[93]Journal of Organometallic Chemistry,2020,vol. 914
[94]Organometallics,2020,vol. 39,p. 1384 - 1392
[95]Russian Chemical Bulletin,2020,vol. 69,p. 492 - 495
    Izv. Akad. Nauk, Ser. Khim.,2020,vol. 69,p. 492 - 495,4
[96]Tetrahedron Letters,2012,vol. 53,p. 5012 - 5014,3
[97]Chemistry - A European Journal,2020,vol. 26,p. 11276 - 11292
[98]New Journal of Chemistry,2020,vol. 44,p. 13934 - 13938
[99]Chemistry - A European Journal,2020,vol. 26,p. 15977 - 15988
[100]Organometallics,2020,vol. 39,p. 4387 - 4394
[101]Journal of Organic Chemistry,2020,vol. 85
[102]Zeitschrift fur Anorganische und Allgemeine Chemie,2021,vol. 647,p. 881 - 895
[103]Chemical Science,2021,vol. 12,p. 3460 - 3474
[104]Molecules,2021,vol. 26
[105]Russian Journal of Coordination Chemistry,2021,vol. 47,p. 546 - 550
    Koord. Khim.,2021,vol. 47,p. 484 - 488
[106]Journal of Organometallic Chemistry,2021,vol. 954-955
[107]ChemistryOpen,2022,vol. 11
  • 3
  • [ 366-18-7 ]
  • [ 14040-11-0 ]
  • [ 15668-66-3 ]
YieldReaction ConditionsOperation in experiment
80% With sodium tetrahydroborate; In butan-1-ol; at 105℃; under 760.051 Torr; for 0.333333h;Microwave irradiation; Inert atmosphere; Green chemistry; General procedure: The reactions were run in a CEM Corp. MARS microwave fitted with a fiber optic temperature probe and a port on top for a reflux condenser.1 mmol of Mo(CO)6 and dppe (0.425 g, 1.1 mmol) were combined with 20 mL of 1-propanol in a two-neck 100 mL RB flask. To this mixture was added NaBH4 (0.128 g, 3.3 mmol). The flaskwas placed in themicrowave and a reflux condenser attached through a hole in the top of the microwave. The mixture was sparged with nitrogen. The mixture was heated under nitrogen at 400 W for 1.5 min to reach reflux temperature. Once the reflux temperature was reached the microwave power was reduced and the temperature maintained for 18 min. The mixture was cooled to room temperature and 2-4 mL of water was added to the reaction to dissolve excess NaBH4 and promote product precipitation. The reaction was cooled -10 C for several hours. The light yellow complex was filtered in air and washed with 2×5 mL of petroleum ether/diethyl ether(1:1) mixture resulting in 580 mg of Mo(CO)4dppe after drying, a 95% yield.
  • 7
  • [ 273-09-6 ]
  • [ 14040-11-0 ]
  • [ 82918-16-9 ]
  • 9
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • [ 75-05-8 ]
  • [ 15228-32-7 ]
  • [ 15096-68-1 ]
  • 10
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • [ 75-05-8 ]
  • [ 15096-68-1 ]
  • 11
  • [ 14040-11-0 ]
  • [ 6737-42-4 ]
  • [ 50860-43-0 ]
YieldReaction ConditionsOperation in experiment
94% With sodium tetrahydroborate; at 120℃; under 760.051 Torr; for 0.666667h;Microwave irradiation; Inert atmosphere; Green chemistry; General procedure: The reactions were run in a CEM Corp. MARS microwave fitted with a fiber optic temperature probe and a port on top for a reflux condenser.1 mmol of Mo(CO)6 and dppe (0.425 g, 1.1 mmol) were combined with 20 mL of 1-propanol in a two-neck 100 mL RB flask. To this mixture was added NaBH4 (0.128 g, 3.3 mmol). The flaskwas placed in themicrowave and a reflux condenser attached through a hole in the top of the microwave. The mixture was sparged with nitrogen. The mixture was heated under nitrogen at 400 W for 1.5 min to reach reflux temperature. Once the reflux temperature was reached the microwave power was reduced and the temperature maintained for 18 min. The mixture was cooled to room temperature and 2-4 mL of water was added to the reaction to dissolve excess NaBH4 and promote product precipitation. The reaction was cooled -10 C for several hours. The light yellow complex was filtered in air and washed with 2×5 mL of petroleum ether/diethyl ether(1:1) mixture resulting in 580 mg of Mo(CO)4dppe after drying, a 95% yield.
  • 13
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • [ 2071-20-7 ]
  • [ 41830-14-2 ]
  • 14
  • [ 14040-11-0 ]
  • [ 1088-00-2 ]
  • [ 114860-50-3 ]
  • [ 114860-49-0 ]
  • 15
  • [ 66-71-7 ]
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • [ 14729-20-5 ]
  • 16
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • [ 15444-65-2 ]
  • 17
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • [ 14586-49-3 ]
  • 18
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • [ 1135-32-6 ]
  • 1,2-bis(4-pyridyl)ethylene ditungsten decacarbonyl [ No CAS ]
  • 19
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • [ 603-35-0 ]
  • [ 15444-65-2 ]
  • 20
  • [ 14040-11-0 ]
  • [ 56-34-8 ]
  • [ 14780-97-3 ]
YieldReaction ConditionsOperation in experiment
In diethylene glycol dimethyl ether; at 120℃; General procedure: Tetraethyl ammonium chloride (0.5 g) was heated with anexcess (1 g) of M(CO)6 (M = Cr, Mo, W) in diethylene glycol ether at 120 C until the steady evolution of carbon monoxide ceased. The mixture was filtered hot under an atmosphere of nitrogen. Adding light petroleum to the cooled filtrate gave yellow crystals of the product. After removal of the excessive solvent by decantation, the crystals were rapidly washed with light petroleum, and the excess of solvent was removed at reduced pressure.
  • 21
  • [ 14040-11-0 ]
  • [ 2426-94-0 ]
  • [ 96211-91-5 ]
  • 22
  • [ 14040-11-0 ]
  • [ 2426-94-0 ]
  • [ 96211-96-0 ]
  • 23
  • [ 10199-00-5 ]
  • [ 14040-11-0 ]
  • [ 80925-51-5 ]
  • 24
  • [ 2044-08-8 ]
  • [ 14040-11-0 ]
  • (CH((CH2)4)C(OCH3))tungsten(carbonyl)5 [ No CAS ]
  • 26
  • [ 4199-89-7 ]
  • [ 14040-11-0 ]
  • [ 59136-53-7 ]
  • [ 201230-82-2 ]
  • 29
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • [ 2071-20-7 ]
  • [ 35324-78-8 ]
  • 30
  • [ 12150-46-8 ]
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • W(CO)4(1,1'-bis(diphenylphosphino)ferrocene) [ No CAS ]
  • W2(CO)10(1,1'-bis(diphenylphosphino)ferrocene)*0.33hexane [ No CAS ]
  • W(CO)5(1,1'-bis(diphenylphosphino)ferrocene) [ No CAS ]
  • 31
  • [ 12150-46-8 ]
  • [ 14040-11-0 ]
  • [ 62637-93-8 ]
  • W(CO)4(1,1'-bis(diphenylphosphino)ferrocene) [ No CAS ]
  • W(CO)5(1,1'-bis(diphenylphosphino)ferrocene) [ No CAS ]
  • 32
  • [ 322-46-3 ]
  • [ 14040-11-0 ]
  • [ 107990-32-9 ]
  • [ 107990-23-8 ]
  • 33
  • [ 322-46-3 ]
  • [ 14040-11-0 ]
  • [ 122780-32-9 ]
  • 34
  • [ 14040-11-0 ]
  • [ 7688-25-7 ]
  • [ 54111-75-0 ]
YieldReaction ConditionsOperation in experiment
75% With sodium tetrahydroborate; at 120℃; under 760.051 Torr; for 0.666667h;Microwave irradiation; Inert atmosphere; Green chemistry; General procedure: The reactions were run in a CEM Corp. MARS microwave fitted with a fiber optic temperature probe and a port on top for a reflux condenser.1 mmol of Mo(CO)6 and dppe (0.425 g, 1.1 mmol) were combined with 20 mL of 1-propanol in a two-neck 100 mL RB flask. To this mixture was added NaBH4 (0.128 g, 3.3 mmol). The flaskwas placed in themicrowave and a reflux condenser attached through a hole in the top of the microwave. The mixture was sparged with nitrogen. The mixture was heated under nitrogen at 400 W for 1.5 min to reach reflux temperature. Once the reflux temperature was reached the microwave power was reduced and the temperature maintained for 18 min. The mixture was cooled to room temperature and 2?4 mL of water was added to the reaction to dissolve excess NaBH4 and promote product precipitation. The reaction was cooled ?10 °C for several hours. The light yellow complex was filtered in air and washed with 2×5 mL of petroleum ether/diethyl ether(1:1) mixture resulting in 580 mg of Mo(CO)4dppe after drying, a 95percent yield.
  • 35
  • [ 14040-11-0 ]
  • [ 19845-69-3 ]
  • [ 120950-74-5 ]
  • 36
  • [ 14040-11-0 ]
  • [ 27721-02-4 ]
  • [ 122991-86-0 ]
  • 37
  • [ 14040-11-0 ]
  • [ 27721-02-4 ]
  • [ 120950-73-4 ]
  • 38
  • [ 14040-11-0 ]
  • (η1-1,1'-bis(diphenylphosphino)ferrocene)Fe(CO)4 [ No CAS ]
  • [ 62637-93-8 ]
  • (CO)4Fe(μ-1,1'-bis(diphenylphosphino)ferrocene)W(CO)5 [ No CAS ]
  • 39
  • [ 14040-11-0 ]
  • [ 557-93-7 ]
  • [ 64-20-0 ]
  • [ 132698-96-5 ]
  • 40
  • [ 14040-11-0 ]
  • [ 136-93-6 ]
  • [ 62637-93-8 ]
  • 2(W(S2CN(C2H5)2)4)(1+)*(W6O19)(2-)=(W(S2CN(C2H5)2)4)2(W6O19) [ No CAS ]
  • 41
  • [ 14040-11-0 ]
  • [ 136-92-5 ]
  • [ 62637-93-8 ]
  • 2(W(S2CN(C2H5)2)4)(1+)*(W6O19)(2-)=(W(S2CN(C2H5)2)4)2(W6O19) [ No CAS ]
  • WSe2(S2CN(C2H5)2)3*0.5H2O [ No CAS ]
  • 42
  • [ 4434-13-3 ]
  • [ 14040-11-0 ]
  • [ 96412-31-6 ]
  • [ 96412-29-2 ]
  • [ 96427-24-6 ]
  • [ 96412-28-1 ]
  • [ 96427-17-7 ]
  • 43
  • [ 14040-11-0 ]
  • [ 96556-05-7 ]
  • [ 98838-67-6 ]
YieldReaction ConditionsOperation in experiment
65% In 1,3,5-trimethyl-benzene; for 2h;Reflux; Inert atmosphere; Schlenk technique; General procedure: 1a was prepared by a modification of the literature method [20,21]. [W(CO)6] (1.5g, 4.3mmol) and Me3tacn (950mg, 5.5mmol) were refluxed in mesitylene (25mL) for 2h under micro-negative pressure, and the reaction was accompanied by the release of CO gas. The reaction flask needs to be covered with a layer of cotton in case of the sublimation of [W(CO)6]. The solution was gradually cooled to room temperature, the yellow solid was filtered off, washed with hot toluene (2×5mL), ethanol (2×5mL), and diethyl ether (2×5mL), successively. The product was recrystallized in dichloromethane and light yellow needle crystals suitable for X-ray crystallographic analysis were collected in two days. Yield: 1.2g (65%). IR (KBr pellets, cm-1): nu(-CH3) 2945(m), nu(-CH2) 2913(m), 2861(s), nu(C?O) 1885(vs), 1750(vs), 1731(vs), nu(C-N) 1449(m). 1H NMR (400MHz, DMSO-d6): delta (ppm) 2.98 (s, 9H, -NCH3), 2.83~2.96 (m, 12H, -NCH2CH2). Anal. (%) Calcd. for C12H21N3O3W: C, 32.79; H, 4.78; N, 9.56. Found: C, 32.80; H, 4.75; N, 9.53.
  • 45
  • [ 1120-88-3 ]
  • [ 14040-11-0 ]
  • (4-methylpyridazine)pentacarbonyltungsten [ No CAS ]
  • 46
  • [ 1132-37-2 ]
  • [ 14040-11-0 ]
  • [ 88814-39-5 ]
  • 47
  • [ 1132-37-2 ]
  • [ 14040-11-0 ]
  • [ 103639-29-8 ]
  • 49
  • [ 14040-11-0 ]
  • [ 6622-92-0 ]
  • W2(2,4-dimethyl-6-oxopyrimidinate)4 [ No CAS ]
  • 50
  • [ 14040-11-0 ]
  • [ 4455-09-8 ]
  • [ 82615-27-8 ]
  • 51
  • [ 14040-11-0 ]
  • [ 665-46-3 ]
  • 3(C2H5)4N(1+)*W2(CO)6F3(3-)=((C2H5)4N)3[W2(CO)6F3] [ No CAS ]
  • 52
  • [ 14040-11-0 ]
  • [ 36802-41-2 ]
  • [ 310871-88-6 ]
  • 53
  • [ 14040-11-0 ]
  • [ 81120-72-1 ]
  • [ 23582-03-8 ]
  • [ 62637-93-8 ]
  • [ 165196-74-7 ]
  • 54
  • [ 14040-11-0 ]
  • [ 12146-36-0 ]
  • [ 62637-93-8 ]
  • [ 23582-02-7 ]
  • [ 165196-71-4 ]
  • 55
  • [ 14040-11-0 ]
  • [ 14667-55-1 ]
  • [ 222017-43-8 ]
  • 56
  • [ 14040-11-0 ]
  • [ 4731-65-1 ]
  • [ 310871-89-7 ]
  • 57
  • [ 67-56-1 ]
  • [ 14040-11-0 ]
  • sodium antimonate [ No CAS ]
  • [ 429-06-1 ]
  • [(C2H5)4N]2[(carbonyl)5WSbW3(carbonyl)9(μ3-methoxy)2(μ3-O)WO2(methoxy)] [ No CAS ]
  • [(C2H5)4N]2[(carbonyl)5WSbW3(carbonyl)9(μ3-methoxy)3WO3] [ No CAS ]
  • 58
  • [ 14040-11-0 ]
  • [ 1867-73-8 ]
  • [ 67-64-1 ]
  • [W(CO)5((N(6)-methyladenosine)] [ No CAS ]
  • 59
  • [ 3438-48-0 ]
  • [ 14040-11-0 ]
  • (4-phenylpyrimidine)pentacarbonyltungsten [ No CAS ]
  • 60
  • [ 41203-22-9 ]
  • [ 14040-11-0 ]
  • cis-[(1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane)W(CO)4] [ No CAS ]
  • 61
  • [ 14040-11-0 ]
  • [ 148461-14-7 ]
  • [W(CO)4((C6H5)2PC6H4CNOCH2CHC3H7)] [ No CAS ]
  • 63
  • [ 36477-75-5 ]
  • [ 368-39-8 ]
  • [ 111770-86-6 ]
  • [ 14040-11-0 ]
  • pentacarbonyl(N-ethyl-3-hydropyridine-1,2-propadienylidene)tungsten [ No CAS ]
  • pentacarbonyl(5-bromo-N-ethyl-3-hydropyridine-1,2-propadienylidene)tungsten [ No CAS ]
  • 64
  • [ 39028-25-6 ]
  • [ 14040-11-0 ]
  • sodium cyclopentadienide [ No CAS ]
  • [ 866529-77-3 ]
  • 66
  • [ 14040-11-0 ]
  • [ 1067-53-4 ]
  • [ 870299-13-1 ]
  • [ 870299-14-2 ]
  • 67
  • [ 14040-11-0 ]
  • [ 580-13-2 ]
  • [ 64-20-0 ]
  • NMe4[(CO)5WC(O)(2-naphthyl)] [ No CAS ]
  • 68
  • [ 14040-11-0 ]
  • [ 831-81-2 ]
  • pentacarbonyl[p-chlorophenyl(phenyl)vinylidene]tungsten [ No CAS ]
  • 69
  • [ 14040-11-0 ]
  • [ 131211-27-3 ]
  • [ 152776-77-7 ]
  • 71
  • [ 14040-11-0 ]
  • [ 16753-62-1 ]
  • [ 870299-09-5 ]
  • [ 870299-10-8 ]
  • 72
  • [ 20112-79-2 ]
  • [ 14040-11-0 ]
  • W(CO)5(2-methylthio-2-imidazoline) [ No CAS ]
  • 73
  • [ 7152-24-1 ]
  • [ 14040-11-0 ]
  • W(CO)5(2-methylthiobenzimidazole) [ No CAS ]
  • 74
  • [ 1826-11-5 ]
  • [ 14040-11-0 ]
  • [ 1225285-45-9 ]
  • 75
  • [ 108-86-1 ]
  • [ 14040-11-0 ]
  • [ 6638-79-5 ]
  • [ 88070-48-8 ]
  • [ 6919-61-5 ]
  • 76
  • [ 104-92-7 ]
  • [ 14040-11-0 ]
  • [ 6638-79-5 ]
  • [ 52898-49-4 ]
  • [ 3400-22-4 ]
  • 77
  • [ 14040-11-0 ]
  • [ 580-13-2 ]
  • [ 6638-79-5 ]
  • [ 113443-62-2 ]
  • 78
  • [ 14040-11-0 ]
  • [ 2551-83-9 ]
  • W(CO)5(E-η2-1-propenylSi(OMe)3) [ No CAS ]
  • W(CO)5(Z-η2-1-propenylSi(OMe)3) [ No CAS ]
  • [ 1194524-63-4 ]
  • [ 1194524-67-8 ]
  • 80
  • [ 14040-11-0 ]
  • [ 110-54-3 ]
  • [ 146960-90-9 ]
  • W(CO)4(1,1'-bis(dicyclohexylphosphino)ferrocene)*0.5(hexane) [ No CAS ]
  • 81
  • [ 97239-80-0 ]
  • [ 14040-11-0 ]
  • [ 1380506-74-0 ]
  • 82
  • [ 29421-92-9 ]
  • [ 14040-11-0 ]
  • [ 368-39-8 ]
  • [W(CO)5{C(OEt)C4H2(Me)S}] [ No CAS ]
  • [W(CO)5{C(OEt)C4HBr(Me)S}] [ No CAS ]
  • [W(CO)4{C(OEt)}2C4H(Me)S] [ No CAS ]
  • 83
  • [ 14040-11-0 ]
  • [ 2071-20-7 ]
  • [ 41830-14-2 ]
YieldReaction ConditionsOperation in experiment
91% With sodium tetrahydroborate; at 120℃; under 760.051 Torr; for 0.666667h;Microwave irradiation; Inert atmosphere; Green chemistry; General procedure: The reactions were run in a CEM Corp. MARS microwave fitted with a fiber optic temperature probe and a port on top for a reflux condenser.1 mmol of Mo(CO)6 and dppe (0.425 g, 1.1 mmol) were combined with 20 mL of 1-propanol in a two-neck 100 mL RB flask. To this mixture was added NaBH4 (0.128 g, 3.3 mmol). The flaskwas placed in themicrowave and a reflux condenser attached through a hole in the top of the microwave. The mixture was sparged with nitrogen. The mixture was heated under nitrogen at 400 W for 1.5 min to reach reflux temperature. Once the reflux temperature was reached the microwave power was reduced and the temperature maintained for 18 min. The mixture was cooled to room temperature and 2-4 mL of water was added to the reaction to dissolve excess NaBH4 and promote product precipitation. The reaction was cooled -10 C for several hours. The light yellow complex was filtered in air and washed with 2×5 mL of petroleum ether/diethyl ether(1:1) mixture resulting in 580 mg of Mo(CO)4dppe after drying, a 95% yield.
  • 84
  • [ 14040-11-0 ]
  • [ 6737-42-4 ]
  • [ 50860-43-0 ]
YieldReaction ConditionsOperation in experiment
94% With sodium tetrahydroborate; at 120℃; under 760.051 Torr; for 0.666667h;Microwave irradiation; Inert atmosphere; Green chemistry; General procedure: The reactions were run in a CEM Corp. MARS microwave fitted with a fiber optic temperature probe and a port on top for a reflux condenser.1 mmol of Mo(CO)6 and dppe (0.425 g, 1.1 mmol) were combined with 20 mL of 1-propanol in a two-neck 100 mL RB flask. To this mixture was added NaBH4 (0.128 g, 3.3 mmol). The flaskwas placed in themicrowave and a reflux condenser attached through a hole in the top of the microwave. The mixture was sparged with nitrogen. The mixture was heated under nitrogen at 400 W for 1.5 min to reach reflux temperature. Once the reflux temperature was reached the microwave power was reduced and the temperature maintained for 18 min. The mixture was cooled to room temperature and 2-4 mL of water was added to the reaction to dissolve excess NaBH4 and promote product precipitation. The reaction was cooled -10 C for several hours. The light yellow complex was filtered in air and washed with 2×5 mL of petroleum ether/diethyl ether(1:1) mixture resulting in 580 mg of Mo(CO)4dppe after drying, a 95% yield.
  • 85
  • [ 14040-11-0 ]
  • [ 7688-25-7 ]
  • [ 54111-75-0 ]
YieldReaction ConditionsOperation in experiment
75% With sodium tetrahydroborate; at 120℃; under 760.051 Torr; for 0.666667h;Microwave irradiation; Inert atmosphere; Green chemistry; General procedure: The reactions were run in a CEM Corp. MARS microwave fitted with a fiber optic temperature probe and a port on top for a reflux condenser.1 mmol of Mo(CO)6 and dppe (0.425 g, 1.1 mmol) were combined with 20 mL of 1-propanol in a two-neck 100 mL RB flask. To this mixture was added NaBH4 (0.128 g, 3.3 mmol). The flaskwas placed in themicrowave and a reflux condenser attached through a hole in the top of the microwave. The mixture was sparged with nitrogen. The mixture was heated under nitrogen at 400 W for 1.5 min to reach reflux temperature. Once the reflux temperature was reached the microwave power was reduced and the temperature maintained for 18 min. The mixture was cooled to room temperature and 2?4 mL of water was added to the reaction to dissolve excess NaBH4 and promote product precipitation. The reaction was cooled ?10 °C for several hours. The light yellow complex was filtered in air and washed with 2×5 mL of petroleum ether/diethyl ether(1:1) mixture resulting in 580 mg of Mo(CO)4dppe after drying, a 95percent yield.
  • 86
  • [ 14040-11-0 ]
  • [ 2071-20-7 ]
  • [ 41830-14-2 ]
YieldReaction ConditionsOperation in experiment
91% With sodium tetrahydroborate; at 120℃; under 760.051 Torr; for 0.666667h;Microwave irradiation; Inert atmosphere; Green chemistry; General procedure: The reactions were run in a CEM Corp. MARS microwave fitted with a fiber optic temperature probe and a port on top for a reflux condenser.1 mmol of Mo(CO)6 and dppe (0.425 g, 1.1 mmol) were combined with 20 mL of 1-propanol in a two-neck 100 mL RB flask. To this mixture was added NaBH4 (0.128 g, 3.3 mmol). The flaskwas placed in themicrowave and a reflux condenser attached through a hole in the top of the microwave. The mixture was sparged with nitrogen. The mixture was heated under nitrogen at 400 W for 1.5 min to reach reflux temperature. Once the reflux temperature was reached the microwave power was reduced and the temperature maintained for 18 min. The mixture was cooled to room temperature and 2-4 mL of water was added to the reaction to dissolve excess NaBH4 and promote product precipitation. The reaction was cooled -10 C for several hours. The light yellow complex was filtered in air and washed with 2×5 mL of petroleum ether/diethyl ether(1:1) mixture resulting in 580 mg of Mo(CO)4dppe after drying, a 95% yield.
  • 87
  • [ 109-72-8 ]
  • [ 14040-11-0 ]
  • [ 5518-52-5 ]
  • [ 368-39-8 ]
  • [ethoxy(2-furyl)carbene]pentacarbonyltungsten(0) [ No CAS ]
  • ((CO)5WC(OC2H5))2C4H2O [ No CAS ]
  • C28H17O15PW2 [ No CAS ]
  • C36H21O21PW3 [ No CAS ]
  • C20H19O8PW [ No CAS ]
  • C20H13O9PW [ No CAS ]
  • 88
  • [ 109-72-8 ]
  • [ 14040-11-0 ]
  • [ 5518-52-5 ]
  • [ 368-39-8 ]
  • [ethoxy(2-furyl)carbene]pentacarbonyltungsten(0) [ No CAS ]
  • C28H17O15PW2 [ No CAS ]
  • C36H21O21PW3 [ No CAS ]
  • C20H19O8PW [ No CAS ]
  • C20H13O9PW [ No CAS ]
  • 89
  • [ 109-72-8 ]
  • [ 14040-11-0 ]
  • [ 5518-52-5 ]
  • [ 368-39-8 ]
  • [ethoxy(2-furyl)carbene]pentacarbonyltungsten(0) [ No CAS ]
  • C20H19O8PW [ No CAS ]
  • C20H13O9PW [ No CAS ]
  • 90
  • [ 14040-11-0 ]
  • [ 696-62-8 ]
  • [ 64-20-0 ]
  • N(CH3)4(1+)*W(CO)5(C(O)C6H4OCH3)(1-)=(N(CH3)4){W(CO)5(C(O)C6H4OCH3)} [ No CAS ]
  • 91
  • [ 14040-11-0 ]
  • [ 368-39-8 ]
  • [ 3958-03-0 ]
  • 5,5,5,5-tetracarbonyl-4,6-diethoxy-5-tungsta(0)cyclopentatrieno[b]thiophene [ No CAS ]
  • C8S(OC2H5)4W2(CO)8 [ No CAS ]
  • 92
  • [ 14040-11-0 ]
  • [ 3958-03-0 ]
  • [ 4111-54-0 ]
  • C16Br2O12SW2(2-)*2Li(1+) [ No CAS ]
  • C10HBr2O6SW(1-)*Li(1+) [ No CAS ]
  • 93
  • [ 3172-56-3 ]
  • [ 14040-11-0 ]
  • [ 368-39-8 ]
  • [ 199620-14-9 ]
  • C24H14CrO12S2W [ No CAS ]
  • C24H14CrO12S2W [ No CAS ]
  • C16H10O6S2W [ No CAS ]
  • C16H10CrO6S2 [ No CAS ]
  • C16H10O6S2W [ No CAS ]
  • C16H10CrO6S2 [ No CAS ]
  • C24H14Cr2O12S2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
57%; 15%; 1% 0.75 g (4.5 mmol) of 3,30-bithiophenewas dissolved in 30 mL THF, 3.10 mL (5.0 mmol) of n-BuLiwas added at -78 C and the reaction mixture stirred for 30 min.Solid portions of 1.58 g (4.5 mmol) W(CO)6 were then added. After15 min of stirring, the solution was removed from the cold bathand stirred for a further 40 min at room temperature. The solutionwas then cooled to -78 C and 3.10 mL (5.0 mmol) of n-BuLi wasadded and the mixture was allowed to stir for 30 min. Solid portionsof 0.99 g (4.5 mmol) Cr(CO)6 were then added. After 15 minof stirring, the solution was removed from the cold bath and stirredfor a further 40 min at room temperature. The solvent wasremoved in vacuo, the reaction residue was dissolved in 10 mLDCM and cooled to -30 C. 1.70 g (9.0 mmol) of [Et3O][BF4] wasdissolved in 10 mL DCM and added to the cold reaction mixturethat was then allowed to rise to room temperature. The mixturewas filtered through a silica gel plug with DCM and the solventremoved at a reduced pressure. Column chromatography yieldedseven complexes. The monocarbene complexes (2b, 1b, 2a and1a) eluted first, followed by the biscarbene complexes (13ab/baand 10b).13ab: Yield: 1.48 g (1.86 mmol, 57%), purple-red crystals.nuCO(hexane)/cm-1 2072w and 2064w (A1(1), W), 2057 m (A1(1), Cr),1987vw (B1, Cr), 1984vw (B1, W), 1961sh (A1(2)), 1955vs (E). delta1H(400.13 MHz; CDCl3; Me4Si): 8.04 (1H, s, H4), 7.19 (1H, dd, 4J2',5' 2.9 and 4J2',4' 1.1, H2'), 6.96 (1H, dd, 3J4',5' 5.0 and 4J4',2' 1.0, H4'),7.36 (1H, dd, 3J5',4' 5.0 and 4J5',2' 3.0, H5'), 4.73 (2H, q, 3J 7.0,C2CH2), 5.21 (2H, q, 3J 7.0, C5CH2), 1.27 (3H, t, 3J 7.1, C2CH3) 1.70(3H, t, 3J 7.0, C5CH3). delta13C(100.613 MHz; CDCl3; Me4Si) 304.6 (CcarbW), 317.7 (Ccarb Cr), 203.0 (COtrans W), 196.6 (COcis W), 223.4(COtrans Cr), 216.6 (COcis Cr), 155.4 (C2), 136.1 (C3), 140.1 (C4),155.4 (C5), 123.1 (C2'), 131.6 (C3'), 127.9 (C4'), 126.0 (C5'), 79.4(CH2 W), 76.4 (CH2 Cr), 14.1 (CH3 W). 15.1 (CH3 Cr). m/z(C24H14O12-S2WCr, 793.88 g/mol) 624.8883 (9%, [M-H-6CO]-), 596.8881(72%, [M-H-7CO]-), 568.8915 (100%, [M-H-8CO]-).13ba: Yield: 0.39 g (0.49 mmol, 15%), purple-red crystals). delta1H(400.13 MHz; CDCl3; Me4Si): 7.97 (1H, s, H4), 7.16 (1H, dd, 4J2',5'2.8 and 4J2',4' 1.0, H2'), 7.00 (1H, dd, 3J4',5' 4.9 and 4J4',2' 1.1, H4'),7.38 (1H, dd, 3J5',4' 5.0 and 4J5',2' 3.0, H5'), 4.73 (2H, q, 3J 7.0,C2CH2), 5.01 (2H, q, 3J 7.0, C5CH2), 1.39 (3H, t, 3J 7.1, C2CH3) 1.68(3H, t, 3J 7.2, C5CH3). delta13C(100.613 MHz; CDCl3; Me4Si) 290.7 (CcarbW), 317.7 (Ccarb Cr), 202.4 (COtrans W), 197.3 (COcis W), 223.8(COtrans Cr), 215.3 (COcis Cr), n.o. (C2), n.o. (C3), 140.0 (C4), n.o.(C5), 123.2 (C2'), n.o. (C3'), 127.5 (C4'), 126.5 (C5'), 78.8 (CH2 W),76.4 (CH2 Cr), 14.9 (CH3 W). 14.6 (CH3 Cr).
  • 94
  • [ 3172-56-3 ]
  • [ 14040-11-0 ]
  • [ 368-39-8 ]
  • C24H14O12S2W2 [ No CAS ]
  • C24H14O12S2W2 [ No CAS ]
  • C19H14O8S2W [ No CAS ]
  • C16H10O6S2W [ No CAS ]
  • C16H10O6S2W [ No CAS ]
  • C24H14O12S2W2 [ No CAS ]
YieldReaction ConditionsOperation in experiment
< 3%; < 3%; < 3%; 34%; 17%; 28% 0.34 g (2.0 mmol) of <strong>[3172-56-3]3,3'-bithiophene</strong> was dissolved in 15 mLTHF, 1.90 mL (3.0 mmol) of n-BuLi and 1.06 g (3.0 mmol) W(CO)6were added. The reaction mixture was later dissolved in 10 mLDCM and 0.8 g (4.0 mmol) [Et3O][BF4], dissolved in 10 mL DCM,was added. Column chromatography yielded six complexes. Compound2a first eluted, followed by 1a, 12a, 11a, 10a and 17a.1a: Yield: 0.37 g (0.68 mmol, 34%), red crystals. nuCO(hexane)/cm-1 2068 m (A1(1)), 1983vw (B1), 1954sh (A1(2)), 1944vs (E). delta1H(300.13 MHz; CDCl3; Me4Si): 7.12 (1H, d, 3J4,5 5.0, H4), 7.71 (1H,d, 3J5,4 5.0, H5), 7.15 (1H, dd, 4J2',5' 3.0 and 4J2',4' 1.3, H2'), 6.94(1H, dd, 3J4',5' 5.0 and 4J4',2' 1.3, H4'), 7.32 (1H, dd, 3J5',4' 5.0 and4J5',2' 3.0, H5'), 4.71 (2H, q, 3J 7.1, CH2), 1.14 (3H, t, 3J 7.1, CH3).delta13C(75.468 MHz; CDCl3; Me4Si) 298.6 (Ccarb), 202.6 (COtrans),197.4 (COcis), 156.8 (C2), 137.8 (C3), 131.6 (C4), 134.1 (C5), 122.4(C2'), 133.5 (C3'), 128.5 (C4'), 125.2 (C5'), 79.0 (CH2), 14.0 (CH3).m/z(C16H10O6S2W, 545.94 g/mol) 566.8801 (96%, [M+Na-2H]-),538.8760 (63%, [M+Na-2H-CO]), 482.9084 (100%, [M+Na-2H-3CO]-).2a: Yield: 0.19 g (0.35 mmol, 17%), red-purple crystals.nuCO(hexane)/cm-1 2067 m (A1(1)), 1981vw (B1), 1954sh (A1(2)),1944vs (E). delta1H(300.13 MHz; CDCl3; Me4Si): 7.83 (1H, d, 4J2,41.3, H2), 8.30 (1H, d, 4J4,2 1.4, H4), 7.46 (1H, dd, 4J2',5' 2.9 and4J2',4' 1.3, H2'), 7.33 (1H, d, 3J4',5' 5.0, H4'), 7.41 (1H, dd, 3J5',4'5.0 and 4J5',2' 2.9, H5'), 5.01 (2H, q, 3J 7.1, CH2), 1.68 (3H, t, 3J7.1, CH3). delta13C(75.468 MHz; CDCl3; Me4Si) 290.6 (Ccarb), 202.4(COtrans), 197.6 (COcis), 130.2 (C2), 139.2 (C3), 138.9 (C4), 158.5(C5), 120.8 (C2'), 136.0 (C3'), 126.0 (C4'), 126.8 (C5'), 78.6(CH2), 15.0 (CH3). m/z(C16H10O6S2W, 545.94 g/mol) 566.8880(75%, [M+Na-2H]-), 538.8806 (45%, [M+Na-2H-CO]-), 482.9099(100%, [M+Na-2H-3CO].10a: Yield: 0.52 g (0.56 mmol, 28%), purple-red crystals.nuCO(hexane)/cm-1 2064 m (A1(1)), 1982vw (B1), 1955sh (A1(2)),1946vs (E). delta1H(300.13 MHz; CDCl3; Me4Si) 7.87 (2H, d, 4J2,4 1.2,H2), 8.30 (2H, d, 4J4,2 1.2, H4), 5.03 (4H, q, 3J 7.0, CH2), 1.69 (6H, t,3J 7.0, CH3). delta13C(75.468 MHz; CDCl3; Me4Si) 290.8 (Ccarb), 202.3(COtrans), 197.5 (COcis), 130.4 (C2), 137.5 (C3), 138.8 (C4), 158.9(C5), 78.7 (CH2), 14.9 (CH3). m/z(C24H14O12S2W2, 925.89 g/mol)924.8770 (20%, [MH]), 868.8815 (48%, [MH2CO]),840.9309 (99%, [MH3CO]), 812.8959 (100%, [MH4CO]-).11a: Yield: <3%, purple-red crystals. delta1H(400.13 MHz; CDCl3;Me4Si): 7.48 (1H, d, 3J4,5 4.3, H4), 8.09 (1H, d, 3J5,4 4.3, H5), 4.99(2H, q, 3J7.1, CH2), 1.68 (3H, t, 3J7.1, CH3).12a: Yield: <3%, purple-red crystals. delta1H(400.13 MHz; CDCl3;Me4Si) 7.10 (1H, d, 3J4,5 5.0, H4), 7.78 (1H, d, 3J5,4 5.0, H5), 7.56(1H, d, 4J2',4' 1.2, H20), 7.90 (1H, d, 4J4',2' 1.2, H40), 4.72 (2H, q, 3J7.1, C2CH2), 5.01 (2H, q, 3J 6.9, C50CH2), 1.16 (3H, t, 3J 7.1,C2CH3), 1.67 (3H, t, 3J 6.9, C50CH3).17a: Yield: <3%, red crystals. delta1H(400.13 MHz; CDCl3; Me4Si)8.02 (1H, s, H4), 7.61 (1H, dd, 4J2',5' 2.9 and 4J2',4' 1.3, H2'), 7.32(1H, dd, 3J4',5' 5.0 and 4J4',2' 1.2, H4'), 7.37 (1H, dd, 3J5',4' 5.0 and4J5',2' 3.0, H5'), 4.32 (2H, q, 3J 7.0, C2-CH2), 5.02 (2H, q, 3J 7.0, C5-CH2), 1.33 (3H, t, 3J 7.2, C2-CH3), 1.70 (3H, t, 3J 7.1, C5-CH3).
  • 95
  • [ 14040-11-0 ]
  • [ 65094-22-6 ]
  • [ 145349-76-4 ]
  • C10H10F2OS [ No CAS ]
  • 96
  • [ 14040-11-0 ]
  • [ 4848-43-5 ]
  • tetracarbonyl(2-(diphenylphosphino)-ethylamine)tungsten(0) [ No CAS ]
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