trichloro(ethenyl)silane

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 500 ml. three-necked flask were charged 108 g. (0.78 mole) 1-phenyl-ethanethiol, 126 g. (0.78 mole) vinyltrichlorosilane and 1.2 g. (0.5 weight percent) azobisisobutyronitrile catalyst. The contents were heated and stirred for 6 hours at 80°-90°C. Fractional distillation of the reaction mixture gave the product fraction, Cl3SiCH2CH2SCH(CH3)C6H5, b.p. 110°/0.53 mm Hg. Vapor phase chromatographic analysis of the distilled product (120 g.) showed it contained a mixture of alpha and beta isomers. Yield of (1-phenylethylthio)ethyltrichlorosilane was 85 percent, based on ViSiCl3 reacted. three-necked flask were charged 108 g The contents were heated Fractional distillation of the reaction mixture

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 86.5 ml. furfuryl alcohol in 200 ml. toluene was slowly added 23 g. sodium metal. An additional 10 ml. furfuryl alcohol was added and the solution was heated to 100° C. with stirring to convert all the sodium. The solution was cooled to ice temperature and 43.5 ml. vinyltrichlorosilane dissolved in 50 ml. toluene was slowly added. After the addition was complete, the mixture was heated at 95° C. for 0.5 hr. The colloidal sodium chloride by-product was extracted with water. The organic phase was filtered and the toluene removed by vacuum evaporation. The residue was distilled at 2 mmHg and the product recovered at 182°-184° C. The solution was cooled to ice temperature and 43.5 ml After the addition the mixture was heated at 95° C. for 0.5 hr The colloidal sodium chloride by-product was extracted with water The organic phase was filtered the toluene removed by vacuum evaporation The residue was distilled at 2 mmHg the product recovered at 182°-184° C.

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 86.5 ml. furfuryl alcohol in 200 ml. toluene was slowly added 23 g. sodium metal. An additional 10 ml. furfuryl alcohol was added and the solution was heated to 100° C. with stirring to convert all the sodium. The solution was cooled to ice temperature and 43.5 ml. vinyltrichlorosilane dissolved in 50 ml. toluene was slowly added. After the addition was complete, the mixture was heated at 95° C. for 0.5 hr. The colloidal sodium chloride by-product was extracted with water. The organic phase was filtered and the toluene removed by vacuum evaporation. The residue was distilled at 2 mmHg and the product recovered at 182°-184° C. The solution was cooled to ice temperature and 43.5 ml After the addition the mixture was heated at 95° C. for 0.5 hr The colloidal sodium chloride by-product was extracted with water The organic phase was filtered the toluene removed by vacuum evaporation The residue was distilled at 2 mmHg the product recovered at 182°-184° C.

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

実験手順: In the same apparatus and by the same procedure described in EXAMPLE 1, n-butylbenzene 0.86 g (6.40 mmol), vinyltrichlorosilane 5.17 g (32.00 mmol) and aluminum chloride 0.047 g (0.35 mmol) were reacted at 80° C. for 6 hours under a dry nitrogen atmosphere. Recrystallization of solid product from THF gave 6.16 g (yield: 2.68%, mp: 228°-35° C.) of pentakis(trichlorosilylethyl)-n-butylbenzene. Distillation of the filtrate gave 2.20 g (yield: 36.59%, bp: 192°-8° C./0.6 mm), 1.81 g (yield: 30.0%, bp: 220°-5° C./0-6 mm), 0.63 g (yield: 10.15%), 0.12 g (yield: 2.05%) and 0.22 g (yield: 3.59%) of tris-, tetrakis(trichlorosilylethyl)-n-butylbenzenes, tetrakis(trichlorosilylethyl)dibutylbenzene, mono- and bis(trichlorosilylethyl)benzenes, respectively. isomeric mixtures were also obtained. NMR data of the polyalkylated products prepared as above are listed in Table 13. were reacted at 80° C. for 6 hours under a dry nitrogen atmosphere Recrystallization of solid product from THF

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 same apparatus and by the same procedure described in EXAMPLE 1, n-butylbenzene 0.86 g (6.40 mmol), vinyltrichlorosilane 5.17 g (32.00 mmol) and aluminum chloride 0.047 g (0.35 mmol) were reacted at 80° C. for 6 hours under a dry nitrogen atmosphere. Recrystallization of solid product from THF gave 6.16 g (yield: 2.68%, mp: 228°-35° C.) of pentakis(trichlorosilylethyl)-n-butylbenzene. Distillation of the filtrate gave 2.20 g (yield: 36.59%, bp: 192°-8° C./0.6 mm), 1.81 g (yield: 30.0%, bp: 220°-5° C./0-6 mm), 0.63 g (yield: 10.15%), 0.12 g (yield: 2.05%) and 0.22 g (yield: 3.59%) of tris-, tetrakis(trichlorosilylethyl)-n-butylbenzenes, tetrakis(trichlorosilylethyl)dibutylbenzene, mono- and bis(trichlorosilylethyl)benzenes, respectively. isomeric mixtures were also obtained. NMR data of the polyalkylated products prepared as above are listed in Table 13. were reacted at 80° C. for 6 hours under a dry nitrogen atmosphere Recrystallization of solid product from THF

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

実験手順: Vinyltrichlorosilane (16.8 g, 104 mmol) was heated to 60° C. and 100 μL 10% H2PtCl6/IPA-solution was added. 1,1,1,4,4-pentachloro-1,4-disilabutane (20.4 g, 77.7 mmol) was added slowly during 20 min so that the temperature did not exceed 100° C. The reaction was allowed to proceed for 12 hours at 100° C., after which it was distilled under vacuum at 115-130° C./<1 mbar. The yield was 31.5 g (74.3 mmol, 96%). did not exceed 100° C after which it was distilled under vacuum at 115-130° C./<1 mbar

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Vinyltrichlorosilane (68.8 g, 426 mmol) and cobalt octacarbonyl (700 mg) were placed in a 100 mL rb flask and cooled in an ice bath to 0° C. Dichlorosilane (bp. 8° C., 44.3 g, 439 mmol) was then condensed into the flask, The system was allowed to warm up to room temperature during night. Distillation at 60 . . . 62° C./8 mbar gave 1,1,1,4,4-Pentachloro-1,4-disilabutane (120.8 g, 460 mmol) in 93% yield. condensed into the flask to warm up to room temperature during night Distillation at 60

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Vinyltrichlorosilane (68.8 g, 426 mmol) and cobalt octacarbonyl (700 mg) were placed in a 100 mL rb flask and cooled in an ice bath to 0° C. Dichlorosilane (bp. 8° C., 44.3 g, 439 mmol) was then condensed into the flask, The system was allowed to warm up to room temperature during night. Distillation at 60 . . . 62° C./8 mbar gave 1,1,1,4,4-Pentachloro-1,4-disilabutane (120.8 g, 460 mmol) in 93% yield. condensed into the flask to warm up to room temperature during night Distillation at 60

反応条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 86.5 ml. furfuryl alcohol in 200 ml. toluene was slowly added 23 g. sodium metal. An additional 10 ml. furfuryl alcohol was added and the solution was heated to 100° C. with stirring to convert all the sodium. The solution was cooled to ice temperature and 43.5 ml. vinyltrichlorosilane dissolved in 50 ml. toluene was slowly added. After the addition was complete, the mixture was heated at 95° C. for 0.5 hr. The colloidal sodium chloride by-product was extracted with water. The organic phase was filtered and the toluene removed by vacuum evaporation. The residue was distilled at 2 mmHg and the product recovered at 182°-184° C. The solution was cooled to ice temperature and 43.5 ml After the addition the mixture was heated at 95° C. for 0.5 hr The colloidal sodium chloride by-product was extracted with water The organic phase was filtered the toluene removed by vacuum evaporation The residue was distilled at 2 mmHg the product recovered at 182°-184° C.

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

実験手順: In the same apparatus and by the same procedure described in EXAMPLE 1, n-butylbenzene 0.86 g (6.40 mmol), vinyltrichlorosilane 5.17 g (32.00 mmol) and aluminum chloride 0.047 g (0.35 mmol) were reacted at 80° C. for 6 hours under a dry nitrogen atmosphere. Recrystallization of solid product from THF gave 6.16 g (yield: 2.68%, mp: 228°-35° C.) of pentakis(trichlorosilylethyl)-n-butylbenzene. Distillation of the filtrate gave 2.20 g (yield: 36.59%, bp: 192°-8° C./0.6 mm), 1.81 g (yield: 30.0%, bp: 220°-5° C./0-6 mm), 0.63 g (yield: 10.15%), 0.12 g (yield: 2.05%) and 0.22 g (yield: 3.59%) of tris-, tetrakis(trichlorosilylethyl)-n-butylbenzenes, tetrakis(trichlorosilylethyl)dibutylbenzene, mono- and bis(trichlorosilylethyl)benzenes, respectively. isomeric mixtures were also obtained. NMR data of the polyalkylated products prepared as above are listed in Table 13. were reacted at 80° C. for 6 hours under a dry nitrogen atmosphere Recrystallization of solid product from THF