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Chemical Structure| 150-60-7 Chemical Structure| 150-60-7
Chemical Structure| 150-60-7

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Product Details of Dibenzyl disulfide

CAS No. :150-60-7
Formula : C14H14S2
M.W : 246.39
SMILES Code : C1(CSSCC2=CC=CC=C2)=CC=CC=C1
English Name :Dibenzyl disulfide
MDL No. :MFCD00004783
InChI Key :GVPWHKZIJBODOX-UHFFFAOYSA-N
Pubchem ID :9012

Safety of Dibenzyl disulfide

Application In Synthesis of Dibenzyl disulfide

* 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 [ 150-60-7 ]

[ 150-60-7 ] Synthesis Path-Downstream   1~36

  • 1
  • [ 150-60-7 ]
  • [ 1184-90-3 ]
  • [ 100-53-8 ]
  • 2
  • [ 538-28-3 ]
  • [ 150-60-7 ]
  • 3
  • [ 150-60-7 ]
  • [ 37493-16-6 ]
  • C3H6LiO(1-)*Li(1+) [ No CAS ]
  • 4
  • [ 150-60-7 ]
  • [ 70264-24-3 ]
  • [ 6345-19-3 ]
  • [ 100-52-7 ]
YieldReaction ConditionsOperation in experiment
In benzene Heating;
  • 5
  • [ 60940-34-3 ]
  • [ 100-53-8 ]
  • [ 150-60-7 ]
  • [ 106663-84-7 ]
  • 6
  • [ 463-58-1 ]
  • [ 24244-54-0 ]
  • [ 150-60-7 ]
  • [ 6972-05-0 ]
  • [ 7250-18-2 ]
  • [ 41948-54-3 ]
YieldReaction ConditionsOperation in experiment
In benzene for 6h; Further byproducts given;
  • 7
  • [ 463-58-1 ]
  • [ 24244-54-0 ]
  • [ 150-60-7 ]
  • [ 7250-18-2 ]
  • [ 41948-54-3 ]
  • [ CAS Unavailable ]
YieldReaction ConditionsOperation in experiment
In benzene Further byproducts given;
  • 8
  • [ 463-58-1 ]
  • [ 24244-54-0 ]
  • [ 150-60-7 ]
  • [ 7250-18-2 ]
  • [ 41948-54-3 ]
  • [ 100-53-8 ]
YieldReaction ConditionsOperation in experiment
In benzene Further byproducts given;
  • 10
  • [ 150-60-7 ]
  • [ 1193-24-4 ]
  • [ 138918-23-7 ]
  • 11
  • [ 7664-41-7 ]
  • [ 538-28-3 ]
  • [ 150-60-7 ]
  • 12
  • [ 64-17-5 ]
  • [ 67-66-3 ]
  • [ 538-28-3 ]
  • phenacyl bromide (1 mol) [ No CAS ]
  • NaHCO3 [ No CAS ]
  • [ 150-60-7 ]
  • [ 2408-88-0 ]
  • [ 6297-94-5 ]
  • [ 247224-05-1 ]
  • 13
  • [ 150-60-7 ]
  • [ 16420-13-6 ]
  • [ 7250-18-2 ]
YieldReaction ConditionsOperation in experiment
67% Stage #1: dibenzyl disulphide With lithium aluminium tetrahydride In tetrahydrofuran at 0℃; for 0.5h; Stage #2: N,N-Dimethylthiocarbamoyl chloride In tetrahydrofuran at 0℃; for 2h;
  • 14
  • [ 98-87-3 ]
  • [ 104347-67-3 ]
  • [ 150-60-7 ]
  • [ 27249-90-7 ]
YieldReaction ConditionsOperation in experiment
1: 39% 2: 36% 3: 6% With sodium sulfide In ethanol Heating;
  • 15
  • [ 150-60-7 ]
  • [ 2217-79-0 ]
  • [ 831-91-4 ]
YieldReaction ConditionsOperation in experiment
78% Stage #1: dibenzyl disulphide With aluminium trichloride; zinc In acetonitrile at 80℃; for 2h; Stage #2: diphenyliodonium iodide In water; acetonitrile at 80℃; for 5h;
  • 16
  • [ 147372-41-6 ]
  • [ 100-53-8 ]
  • [ 333454-24-3 ]
  • [ 150-60-7 ]
YieldReaction ConditionsOperation in experiment
2.45 g With sodium In ethanol at 20℃; for 16h;
  • 17
  • [ 42275-47-8 ]
  • [ 100-53-8 ]
  • [ 150-60-7 ]
  • [ 87122-96-1 ]
YieldReaction ConditionsOperation in experiment
4.28 g With sodium In ethanol at 20℃; for 16h;
  • 18
  • [ 150-60-7 ]
  • [ 61259-29-8 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 3 steps 1.1: 95 percent / I2 / CH2Cl2 / 22 h / 20 °C 2.1: iPrMgCl*LiCl / tetrahydrofuran / 1.5 h / -40 °C 2.2: 70 percent / tetrahydrofuran / 0.75 h / -40 - -15 °C
  • 19
  • [ 150-60-7 ]
  • [ 2460-77-7 ]
  • [ CAS Unavailable ]
  • [ CAS Unavailable ]
  • [ CAS Unavailable ]
YieldReaction ConditionsOperation in experiment
1: 58% 2: 85% In toluene (Ar); stirring (-78°C), warming (room temp.), stirring (1 h), addn. (acetonitrile); solid removing, soln. condensation, recrystn. (n-hexane, -78°C) and supernatant pptn. (MeCN); elem. anal.;
  • 20
  • [ 110-81-6 ]
  • [ 150-60-7 ]
  • [ 2179-57-9 ]
  • [ 624-92-0 ]
  • [ 629-19-6 ]
  • [ 20333-39-5 ]
  • [ 2179-60-4 ]
  • [ 30453-31-7 ]
  • [ 2179-59-1 ]
  • [ 72437-63-9 ]
  • [ 21230-16-0 ]
  • [ 27657-11-0 ]
  • [ 2179-58-0 ]
  • [ 699-10-5 ]
  • [ 68794-86-5 ]
YieldReaction ConditionsOperation in experiment
With tricyclohexylphosphine In dimethyl sulfoxide at 20℃;
  • 21
  • [ 150-60-7 ]
  • [ 610791-05-4 ]
  • [ 1340481-85-7 ]
  • 22
  • [ 5350-41-4 ]
  • [ 150-60-7 ]
  • 23
  • [ 150-60-7 ]
  • [ 326-64-7 ]
  • 2-(benzylsulfanyl)-4-chlorophenyl trifluoromethyl ether [ No CAS ]
YieldReaction ConditionsOperation in experiment
51% With isopentyl nitrite; In acetonitrile; at 60℃; for 2h; To a suspension of 5-chloro-2- ( trifluorometnyl ) aniline (5.00 g, 23.6 mmol) and dibenzyl disulfide (4.66g, 18.9 mmol) in acetonitrile (75 mL) , Isoamyl nitrite (3.46 mL, 26.0 mmol) was slowly added at 60C in an oil bath, and the mixture was stirred at the same temperature as above for 2 hours. The reaction mixture was cooled and then concentrated under reduced pressure, and the residue was purified in an automatic chromatography apparatus (n-hexane/ethyl acetate = 100/0 - 95/5) to prepare 2- (benzylsulfanyl ) -4-chlorophenyl trifluoromethyl ether (3.86 g, yield: 51%) . To a mixture of the obtained 2- (benzylsulfanyl ) -4-chlorophenyl trifluoromethyl ether (4.84 g, 15.2 mmol), acetic acid(4.5 mL) and water (3 mL) in acetonitrile (120 mL) , 1, 3-dichloro-5, 5-dimethylhydantoin (5.98 g, 30.4 mmol) was added under ice cooling, and the mixture was stirred at the same temperature as above for 3 hours. The mixture was diluted by addition of a saturated aqueous solution of sodium bicarbonate, extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure, and the residue was purified in an automatic chromatography apparatus(hexane/ethyl acetate = 100/0 - 85/15) to obtain the title compound (3.64 g, yield: 81%) . NMR spectrum (CDC13, 400MHz) delta: 8.09 (1H, d, J =2.3 Hz), 7.75 (1H, dd, J = 9.0, 2.7 Hz), 7.50-7.47 (1H, m) .
51% With isopentyl nitrite; In acetonitrile; at 20 - 60℃; for 2h; To a suspension of 5-chloro-2- (trifluoromethoxy)aniline (5.00 g, 23.6 mmol) and dibenzyl disulfide (4.66g, 18.9 mmol) in acetonitrile (75 mL), isoamyl nitrite (3.46 mL, 26.0 mmol) was slowly added at 60C in an oil bath, and the mixture was stirred at the same temperature as above for 2 hours. The reaction mixture was cooled and then concentrated under reduced pressure, and the residue was purified in an automatic chromatography apparatus (n-hexane/ethyl acetate = 100/0 - 95/5) to prepare 2-(benzylsulfanyl)-4- chlorophenyl trifluoromethyl ether (3.86 g, yield: 51%) To a mixture of 2-(benzylsulfanyl)-4-chlorophenyl trifluoromethyl ether (4.84 g, 15.2 mmol) obtained in the above step, acetic acid (4.5 mL) and water (3 mL) in acetonitrile (l2OmL), 1,3-dichloro-5,5-dimethylhydantoin (5.98 g, 30.4 mmol) was added under ice cooling, and the mixture was stirred at the same temperature as above for 3 hours. The mixture was diluted by addition of a saturated aqueous solution of sodium bicarbonate, extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure, and the residue was purified in an automatic chromatography apparatus (hexane/ethyl acetate = 100/0 - 85/15) to obtain the title compound (3.64 g, yield: 81%) ?H NNR spectrum (CDC13, 400MHz) oe: 8.09 (1H, d, J =2.3 Hz), 7.75 (1H, dd, J = 9.0, 2.7 Hz), 7.50-7.47 (1H, m)
  • 24
  • [ 150-60-7 ]
  • [ 104-94-9 ]
  • [ 5310-26-9 ]
YieldReaction ConditionsOperation in experiment
77% With N-methylcyclohexylamine; sulfur; dimethyl sulfoxide at 100℃; for 16h; Inert atmosphere;
  • 25
  • [ 150-60-7 ]
  • [ 98-32-8 ]
  • 2-phenylbenzoxazole-5-sulfonamide [ No CAS ]
  • 26
  • [ 150-60-7 ]
  • [ 434-42-4 ]
  • [ 2545942-17-2 ]
YieldReaction ConditionsOperation in experiment
47% With palladium diacetate; caesium carbonate; triphenylphosphine; zinc In water; N,N-dimethyl-formamide at 80℃; for 12h; 12 23.8 mg (0.1 mmol) (1-bromo-2,2,2-trifluoroethyl)benzene, 12.3 mg (0.05 mmol) dibenzyl disulfide, 2.2 mg (0.01 mmol) palladium acetate, 26.2 mg (0.1 mmol) triphenylphosphine, 42.4 mg (0.15 mmol) cesium carbonate, 13.0 mg (0.2 mmol) of zinc powder and 14.4 mg (0.8 mmol) of deionized water were added to 2 ml of solvent N,N-dimethylformamide. The reaction was stirred at 80 °C for 12 hours. After the reaction was completed, it was cooled, the mixture was poured into ethyl acetate, and washed with saturated brine (2×15 mL). After extracting the aqueous layer with ethyl acetate, the combined organic layer was dried with anhydrous Na2SO4, filtered and the filtrate was removed from the solvent with a rotary evaporator to obtain the residue. The residue was subjected to column layer separation through a silica gel column and passed through the eluent After washing, the effluent containing the target product is collected, the effluents are combined and concentrated in vacuo to remove the solvent to obtain the target product. The residue is eluted with petroleum ether eluent through a silica gel column, and the effluent is collected according to the actual gradient. TLC detection, combined the effluent containing the product, the rotary evaporator distilled to remove the solvent, vacuum dried to obtain a colorless liquid, benzyl (1-fluoro-2-phenylvinyl) sulfide 11.4 mg, a yield of 47%.
  • 27
  • [ 150-60-7 ]
  • [ 892845-59-9 ]
  • [ 2864804-42-0 ]
YieldReaction ConditionsOperation in experiment
Multi-step reaction with 2 steps 1.1: diisopropylamine; n-butyllithium / tetrahydrofuran; hexane / 2 h / -78 °C / Inert atmosphere 1.2: 1 h / -78 °C / Inert atmosphere 2.1: triethylamine; C47H37ClP2Pd / 3 h / 100 °C / 3750.38 Torr / Sealed tube; Inert atmosphere
  • 28
  • [ 150-60-7 ]
  • [ 892845-59-9 ]
  • [ 2864804-41-9 ]
YieldReaction ConditionsOperation in experiment
56 % Stage #1: 1-bromo-2-chloro-4-(trifluoromethoxy)benzene With n-butyllithium; diisopropylamine In tetrahydrofuran; hexane at -78℃; Inert atmosphere; Stage #2: dibenzyl disulphide In tetrahydrofuran; hexane at -78℃; Inert atmosphere; 1.1 Step 1: Preparation of 3-benzylsulfanyl-1-bromo-2-chloro-4-(trifluoromethoxy)benzene To a 3 necked flask, equipped with a thermometer, containing tetrahydrofuran (200 mL) (that was purged and filled with N2) was added diisopropylamine (6.68 g, 9.30 mL, 65.3 mmol) . The reaction was stirred at -78 °C using a dry ice/acetone bath for 30 min. n-Butyllithium in hexane (2.5 M, 23 mL, 58.1 mmol) was added dropwise, maintaining the temperature at -78 °C and stirred for 40 min. A solution of 1-bromo-2-chloro-4-(trifluoromethoxy)benzene (10.0 g, 36.3 mmol) made up to 20 mL by addition of THF was added dropwise, maintaining the temperature at -78 °C and stirred for 2hr. Benzyldisulfanyl)methylbenzene (17.9 g, 72.6 mmol) in THF (30 mL) is added dropwise and the mixture was stirred at -78 °C for 1 h. Whilst still cold, the reaction mixture was quenched by adding it into a stirred solution of iced water. 2 M HCl was added to acidify the solution and followed by Ethyl acetate extraction x 3. The organic phase was concentrated in vacuo and purified by flash column chromatography (0-10% gradient of EtOAc in cyclohexane).Product-containing fractions were combined and partitioned with 1M NaOH, this added purification step removes the impurity phenylmethanethiol. The organics are again collected and concentrated in vacuo to afford 3-benzylsulfanyl-1-bromo-2-chloro-4-(trifluoromethoxy)benzene (8.5 g, 21 mmol, 56%) as a yellow oil. 1H NMR (CDCl3): 7.59 (d, 1H), 7.25-7.18 (m, 5H), 7.05 (m, 1H), 4.09 (s, 2H)
56 % Stage #1: 1-bromo-2-chloro-4-(trifluoromethoxy)benzene With n-butyllithium; diisopropylamine In tetrahydrofuran; hexane at -78℃; Inert atmosphere; Stage #2: dibenzyl disulphide In tetrahydrofuran; hexane at -78℃; Inert atmosphere; 1.1 Step 1: Preparation of 3-benzylsulfanyl-1-bromo-2-chloro-4-(trifluoromethoxy)benzene To a 3 necked flask, equipped with a thermometer, containing tetrahydrofuran (200 mL) (that was purged and filled with N2) was added diisopropylamine (6.68 g, 9.30 mL, 65.3 mmol) . The reaction was stirred at -78 °C using a dry ice/acetone bath for 30 min. n-Butyllithium in hexane (2.5 M, 23 mL, 58.1 mmol) was added dropwise, maintaining the temperature at -78 °C and stirred for 40 min. A solution of 1-bromo-2-chloro-4-(trifluoromethoxy)benzene (10.0 g, 36.3 mmol) made up to 20 mL by addition of THF was added dropwise, maintaining the temperature at -78 °C and stirred for 2hr. Benzyldisulfanyl)methylbenzene (17.9 g, 72.6 mmol) in THF (30 mL) is added dropwise and the mixture was stirred at -78 °C for 1 h. Whilst still cold, the reaction mixture was quenched by adding it into a stirred solution of iced water. 2 M HCl was added to acidify the solution and followed by Ethyl acetate extraction x 3. The organic phase was concentrated in vacuo and purified by flash column chromatography (0-10% gradient of EtOAc in cyclohexane).Product-containing fractions were combined and partitioned with 1M NaOH, this added purification step removes the impurity phenylmethanethiol. The organics are again collected and concentrated in vacuo to afford 3-benzylsulfanyl-1-bromo-2-chloro-4-(trifluoromethoxy)benzene (8.5 g, 21 mmol, 56%) as a yellow oil. 1H NMR (CDCl3): 7.59 (d, 1H), 7.25-7.18 (m, 5H), 7.05 (m, 1H), 4.09 (s, 2H)
56 % Stage #1: 1-bromo-2-chloro-4-(trifluoromethoxy)benzene With n-butyllithium; diisopropylamine In tetrahydrofuran; hexane at -78℃; Inert atmosphere; Stage #2: dibenzyl disulphide In tetrahydrofuran; hexane at -78℃; Inert atmosphere; 1.1 Step 1: Preparation of 3-benzylsulfanyl-1-bromo-2-chloro-4-(trifluoromethoxy)benzene To a 3 necked flask, equipped with a thermometer, containing tetrahydrofuran (200 mL) (that was purged and filled with N2) was added diisopropylamine (6.68 g, 9.30 mL, 65.3 mmol) . The reaction was stirred at -78 °C using a dry ice/acetone bath for 30 min. n-Butyllithium in hexane (2.5 M, 23 mL, 58.1 mmol) was added dropwise, maintaining the temperature at -78 °C and stirred for 40 min. A solution of 1-bromo-2-chloro-4-(trifluoromethoxy)benzene (10.0 g, 36.3 mmol) made up to 20 mL by addition of THF was added dropwise, maintaining the temperature at -78 °C and stirred for 2hr. Benzyldisulfanyl)methylbenzene (17.9 g, 72.6 mmol) in THF (30 mL) is added dropwise and the mixture was stirred at -78 °C for 1 h. Whilst still cold, the reaction mixture was quenched by adding it into a stirred solution of iced water. 2 M HCl was added to acidify the solution and followed by Ethyl acetate extraction x 3. The organic phase was concentrated in vacuo and purified by flash column chromatography (0-10% gradient of EtOAc in cyclohexane).Product-containing fractions were combined and partitioned with 1M NaOH, this added purification step removes the impurity phenylmethanethiol. The organics are again collected and concentrated in vacuo to afford 3-benzylsulfanyl-1-bromo-2-chloro-4-(trifluoromethoxy)benzene (8.5 g, 21 mmol, 56%) as a yellow oil. 1H NMR (CDCl3): 7.59 (d, 1H), 7.25-7.18 (m, 5H), 7.05 (m, 1H), 4.09 (s, 2H)
  • 29
  • [ 150-60-7 ]
  • [ 217096-31-6 ]
  • [ 2930044-33-8 ]
YieldReaction ConditionsOperation in experiment
27% With isopentyl nitrite In acetonitrile at 80℃; for 2h;
26.7% With Isovaleronitrile In acetonitrile at 70℃; for 1h; 85.3; 86.3 Synthesis of 3-(benzylthio)-2,4-dimethoxypyridine (118) To a stirred solution of compound 117 (3 g, 19.459 mmol) in ACN (30 mL) wasadded 1,2-dibenzyldisulfane (5.60 g, 22.76 mmol) followed by the addition of isoamyl nitrite(6.30 mL). The resulting mixture was stirred at 70 for 1h. After completion (monitored byTLC), the mixture was quenched with ice-cold water and extracted with EtOAc. Thecombined organic layer was washed with brine, dried over anhydrous Na2SO4 andconcentrated under reduced pressure. The crude was purified by combi-flash chromatographyusing 30% EtOAc/Heptane to afford title compound 118 (1.40 g, 26.70%) as a light brownliquid. LCMS calculated for C14H15NO2S: 261.08; Found: 262.10 (M+1).
27 % With isopentyl nitrite In acetonitrile at 80℃; 2.3 Step 3: To a solution of 2-3 (650 mg, 4.22 mmol) in acetonitrile (10 mL) was added 2-4 (1.25 g, 5.06 mmol) and isopentyl nitrite (1.39 mL, 9.28 mmol) at 80 . This reaction mixture was stirred at 80 for 2 h. The reaction mixture was concentrated in vacuum to give a residue which was purified by flash silica gel chromatography to afford 2-5 (300 mg, 27%yield) as a brown oil. LCMS: 262.3 [M+H]+.
27 % With isopentyl nitrite In acetonitrile at 80℃; 2.3 Step 3: To a solution of 2-3 (650 mg, 4.22 mmol) in acetonitrile (10 mL) was added 2-4 (1.25 g, 5.06 mmol) and isopentyl nitrite (1.39 mL, 9.28 mmol) at 80 . This reaction mixture was stirred at 80 for 2 h. The reaction mixture was concentrated in vacuum to give a residue which was purified by flash silica gel chromatography to afford 2-5 (300 mg, 27%yield) as a brown oil. LCMS: 262.3 [M+H]+.
27 % With isopentyl nitrite In acetonitrile at 80℃; 2.3 Step 3: To a solution of 2-3 (650 mg, 4.22 mmol) in acetonitrile (10 mL) was added 2-4 (1.25 g, 5.06 mmol) and isopentyl nitrite (1.39 mL, 9.28 mmol) at 80 . This reaction mixture was stirred at 80 for 2 h. The reaction mixture was concentrated in vacuum to give a residue which was purified by flash silica gel chromatography to afford 2-5 (300 mg, 27%yield) as a brown oil. LCMS: 262.3 [M+H]+.

  • 30
  • [ 150-60-7 ]
  • [ 90197-37-8 ]
  • [ 2930044-82-7 ]
YieldReaction ConditionsOperation in experiment
27% With ascorbic acid; isopentyl nitrite In acetonitrile at 0 - 25℃; for 12h;
27% With ascorbic acid; isopentyl nitrite In acetonitrile at 0 - 25℃; for 12h;
27 % With ascorbic acid; isopentyl nitrite In acetonitrile at 0 - 25℃; 11.1 Step 1: To a mixture of 11-1 (10.0 g, 59.5 mmol) in MeCN (100 mL) were added dibenzyl disulfide (29.3 g, 119 mmol) and L (+) -Ascorbic acid (5.24 g, 29.8 mmol) . Then isoamyl nitrite (25.8 g, 220 mmol) was added to this reaction mixture at 0 and the reaction mixture was stirred at 25 for 12 h. This reaction mixture was concentrated under reduced pressure and the obtained residue was purified by flash silica gel chromatography to afford 11-2(4.4 g, 27%yield) as a yellow oil. LCMS: 276.1 [M+H]+.
27 % With ascorbic acid; isopentyl nitrite In acetonitrile at 0 - 25℃; 11.1 Step 1: To a mixture of 11-1 (10.0 g, 59.5 mmol) in MeCN (100 mL) were added dibenzyl disulfide (29.3 g, 119 mmol) and L (+) -Ascorbic acid (5.24 g, 29.8 mmol) . Then isoamyl nitrite (25.8 g, 220 mmol) was added to this reaction mixture at 0 and the reaction mixture was stirred at 25 for 12 h. This reaction mixture was concentrated under reduced pressure and the obtained residue was purified by flash silica gel chromatography to afford 11-2(4.4 g, 27%yield) as a yellow oil. LCMS: 276.1 [M+H]+.
27 % With ascorbic acid; isopentyl nitrite In acetonitrile at 0 - 25℃; 11.1 Example 11: Synthesis of N-(6-((1H-pyrazol-1-yl)methyl)-4-methoxybenzo[d]isoxazol-3-yl)-2,4-dimethoxy-6-methylpyridine-3-sulfonamide (Compound 11) Step 1: To a mixture of 11-1 (10.0 g, 59.5 mmol) in MeCN (100 mL) were added dibenzyl disulfide (29.3 g, 119 mmol) and L (+) -Ascorbic acid (5.24 g, 29.8 mmol) . Then isoamyl nitrite (25.8 g, 220 mmol) was added to this reaction mixture at 0 and the reaction mixture was stirred at 25 for 12 h. This reaction mixture was concentrated under reduced pressure and the obtained residue was purified by flash silica gel chromatography to afford 11-2(4.4 g, 27%yield) as a yellow oil. LCMS: 276.1 [M+H]+.

  • 31
  • [ 27249-90-7 ]
  • [ 150-60-7 ]
  • [ 7459-69-0 ]
YieldReaction ConditionsOperation in experiment
With carbon disulfide; tetrabutylammonium nitrite In acetonitrile at 20℃; Inert atmosphere;
  • 32
  • [ 2943-26-2 ]
  • [ 150-60-7 ]
YieldReaction ConditionsOperation in experiment
18 % In dimethyl sulfoxide at 100℃;
  • 33
  • [ 36331-57-4 ]
  • [ 150-60-7 ]
YieldReaction ConditionsOperation in experiment
63% With (1,3-dimethyl-1H-benzo[d]imidazol-3-ium-2-yl)trihydroborate In toluene at 140℃; for 12h; Schlenk technique; Inert atmosphere;
63% With (1,3-dimethyl-1H-benzo[d]imidazol-3-ium-2-yl)trihydroborate In toluene at 140℃; for 12h; Inert atmosphere; 19 Preparation Example 19 Add 0.2mmol of sulfonamide compound IV to a 10mL reaction tube, toluene as solvent (0.5mL), 5mol% NHC-BH3 as catalyst (VI), reaction conditions of 140, and reaction for 12h under nitrogen environment. After the reaction, 1,2-dibenzyldisulfane (R = benzyl) was obtained by column chromatography to obtain a colorless solid with a yield of 63%.
  • 34
  • [ 100-44-7 ]
  • [ 1205-17-0 ]
  • [ 150-60-7 ]
  • [ 3098057-46-3 ]
YieldReaction ConditionsOperation in experiment
85% With sulphur; tetrakis(tetrabutylammonium)decatungstate(VI); <i>N</i>,<i>N</i>-dimethyl-aniline In acetonitrile at 25℃; for 12h; Inert atmosphere; Sealed tube; Irradiation; Green chemistry;
  • 35
  • [ 150-60-7 ]
  • [ 21324-39-0 ]
  • [ 22980-76-3 ]
  • [ CAS Unavailable ]
  • [ CAS Unavailable ]
YieldReaction ConditionsOperation in experiment
65% Stage #1: sodium hexaflorophosphate; {Ni(phen)Cl2} In acetonitrile at 20℃; for 0.25h; Inert atmosphere; Schlenk technique; Stage #2: dibenzyl disulphide; potassium <i>tert</i>-butylate In methanol; toluene; acetonitrile for 8h; Inert atmosphere; Schlenk technique; 2.2.1.Synthesis of [Ni{L1}2(Phen)] (1a) General procedure: To an acetonitrile solution (15 mL) of [NiCl2(Phen)] (100 mg, 0.32 mmol), NaPF6 (107.5 mg, 0.64 mmol) was added to it. The reaction mixture was stirred for 15 min at room temperature in an inert atmosphere. The supernatant was added to a solution of NaSC4H(4,6-Me)N2 [prepared from bis-4,6-dimethylpyrimidin-2-yl disulfide (88.9 mg, 0.32 mmol) and sodium borohydride (24.2 mg, 0.64 mmol) in toluene- methanol solution]. The stirring was continued for 8 h. The reaction mixture was dried under vacuum and resulted compound was washed with diethyl ether and hexane. The residue was extracted in acetonitrile which on slow evaporation gave red crystals of title complex
  • 36
  • [ 150-60-7 ]
  • [ 21324-39-0 ]
  • [ 22775-90-2 ]
  • [ CAS Unavailable ]
  • [ CAS Unavailable ]
YieldReaction ConditionsOperation in experiment
68% Stage #1: sodium hexaflorophosphate; dichloro(2,2'-bipyridine)nickel(II) In acetonitrile at 20℃; for 0.25h; Inert atmosphere; Schlenk technique; Stage #2: dibenzyl disulphide; potassium <i>tert</i>-butylate In methanol; toluene; acetonitrile for 8h; Inert atmosphere; Schlenk technique; 2.2.1.Synthesis of [Ni{L1}2(Phen)] (1a) General procedure: To an acetonitrile solution (15 mL) of [NiCl2(Phen)] (100 mg, 0.32 mmol), NaPF6 (107.5 mg, 0.64 mmol) was added to it. The reaction mixture was stirred for 15 min at room temperature in an inert atmosphere. The supernatant was added to a solution of NaSC4H(4,6-Me)N2 [prepared from bis-4,6-dimethylpyrimidin-2-yl disulfide (88.9 mg, 0.32 mmol) and sodium borohydride (24.2 mg, 0.64 mmol) in toluene- methanol solution]. The stirring was continued for 8 h. The reaction mixture was dried under vacuum and resulted compound was washed with diethyl ether and hexane. The residue was extracted in acetonitrile which on slow evaporation gave red crystals of title complex
 

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