dichloro(diphenyl)silane

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In the manner described in Examples 1-7, diphenyldichlorosilane was reacted with about two moles of methyl 3,5,6-trichloro-2-pyridyl carbonate in the presence of tetrabutylammonium chloride to produce a good yield of diphenyl bis(3,5,6-trichloro-2-pyridyloxy)silane, a crystalline solid.

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a suspension of 2-bromotriphenylene (7.28 g, 23.70 mmol) in ether (50 mL) was added n-butyllithium solution in hexane (14.81 mL, 23.70 mmol) dropwise at −78° C. The suspension was gradually warmed to 0° C. and stirred for 3 hours to yield a solution of triphenylenyllithium. In a separate flask a solution of 3-bromophenyllithium was prepared by dropwise addition of n-butyllithium solution in hexane (14.81 mL, 23.70 mmol) into a solution of 1,3-dibromobenzene (2.87 mL, 23.70 mmol) in ether (50 mL). The solution was stirred at this temperature for 2.5 hours before being transferred into a solution of dichlorodiphenylsilane (4.88 mL, 23.70 mmol) in ether (30 mL) at −78° C. After stirring for another 2 h, the triphenylenyllithium solution prepared above was introduced dropwise into the flask containing the dichlorophenylsilane. The reaction mixture was allowed to gradually warm to room temperature and was stirred overnight. The mixture was quenched with water and the organic phase was isolated. Upon evaporation of the solvent, the residue was purified by column chromatography on silica gel with hexane/DCM (85/15, v/v) as eluent to yield (3-bromophenyl)diphenyl(triphenylen-2-yl)silane (8.5 g, 75%) as a white powder. After stirring for another 2 h above was introduced dropwise into the flask was stirred overnight The mixture was quenched with water the organic phase was isolated Upon evaporation of the solvent the residue was purified by column chromatography on silica gel with hexane/DCM (85/15

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a suspension of 2-bromotriphenylene (7.28 g, 23.70 mmol) in ether (50 mL) was added n-butyllithium solution in hexane (14.81 mL, 23.70 mmol) dropwise at −78° C. The suspension was gradually warmed to 0° C. and stirred for 3 hours to yield a solution of triphenylenyllithium. In a separate flask a solution of 3-bromophenyllithium was prepared by dropwise addition of n-butyllithium solution in hexane (14.81 mL, 23.70 mmol) into a solution of 1,3-dibromobenzene (2.87 mL, 23.70 mmol) in ether (50 mL). The solution was stirred at this temperature for 2.5 hours before being transferred into a solution of dichlorodiphenylsilane (4.88 mL, 23.70 mmol) in ether (30 mL) at −78° C. After stirring for another 2 h, the triphenylenyllithium solution prepared above was introduced dropwise into the flask containing the dichlorophenylsilane. The reaction mixture was allowed to gradually warm to room temperature and was stirred overnight. The mixture was quenched with water and the organic phase was isolated. Upon evaporation of the solvent, the residue was purified by column chromatography on silica gel with hexane/DCM (85/15, v/v) as eluent to yield (3-bromophenyl)diphenyl(triphenylen-2-yl)silane (8.5 g, 75%) as a white powder. After stirring for another 2 h above was introduced dropwise into the flask was stirred overnight The mixture was quenched with water the organic phase was isolated Upon evaporation of the solvent the residue was purified by column chromatography on silica gel with hexane/DCM (85/15

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a 3-necked flask equipped with a stirrer, reflux condenser and a gas conduit, is introduced over a period of 5 minutes with constant agitation and at room temperature, 2-liters [measured at 20° C. and 720 mm Hg (abs.) and thus 0.94 percent based on the total weight of the silanes used], of gaseous hydrogen chloride, into a mixture consisting of 253 grams (1 mol) of diphenyldichlorosilane, 88 grams (1 mol) of tetramethylsilane, 3 grams of trichlorosilane and 3 grams diethylaluminum chloride. Stirring is continued for an additional 4 hours while the mixture is heated under reflux. Fractional distillation yields 30 grams of trimethylchlorosilane, 35 grams of phenyldimethylchlorosilane, 80 grams of diphenylmethylchlorosilane and 74 grams of triphenylchlorosilane. Into a 3-necked flask equipped with a stirrer reflux condenser a gas conduit, is introduced over a period of 5 minutes with constant agitation and at room temperature measured at 20° C. is heated under reflux Fractional distillation

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Triethylamine (3.9 g) was added to a flask containing 83.3 g of the crude product mixture described in Example 1. This mixture was stripped by the process described in Example 1. The volatiles were condensed and analyzed by GC-TCD. About 77.4 g of a liquid was recovered comprising 24.7 g of diphenyldichlorosilane (yield of 77 percent), 1.4 g of phenyldichlorosilane, 24.5 g of phenyltrichlorosilane, and 10.1 g of benzene. condensed About 77.4 g of a liquid was recovered

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Example 1 was repeated using 2.27 g. (9 m mols) of diphenyldichlorosilane, 1.0 g. (8.6 m mols) of t-butylacetate and 0.07 g. of tetrabutylammonium bromide, except that the reaction mass was heated at 200° C. for 3 hours. A 48% conversion to t-butyl chloride and a 15% conversion to CH3COCl was obtained.