trichloro(trichlorosilylmethyl)silane

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 procedure as Example 1 above, 0.20 g (0.75 mmol) of triphenylphosphine, 0.92 g (7.5 mmol) of (chloromethyl)trichlorosilane, and 5.08 g (37.5 mmol) of trichlorosilane were reacted at 150° C. for 42 hrs. The resulting mixture was distilled to give 1.1 g of 1,1,1,3,3,3-hexachloro-1,3-disilapropane (bp; 173-174° C., yield; 50%) and 0.3 g of 1,1,1,3,3-pentachloro-1,3-disilapropane (bp; 166-167° C., yield; 16%). The resulting mixture was distilled

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 procedure as Example 1 above, 0.20 g (0.75 mmol) of triphenylphosphine, 0.92 g (7.5 mmol) of (chloromethyl)trichlorosilane, and 5.08 g (37.5 mmol) of trichlorosilane were reacted at 150° C. for 42 hrs. The resulting mixture was distilled to give 1.1 g of 1,1,1,3,3,3-hexachloro-1,3-disilapropane (bp; 173-174° C., yield; 50%) and 0.3 g of 1,1,1,3,3-pentachloro-1,3-disilapropane (bp; 166-167° C., yield; 16%). The resulting mixture was distilled

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 procedure as Example 1 above, 0.22 g (0.67 mmol) of benzyltributylphosphonium chloride, 1.23 g (6.69 mmol) of (chloromethyl)trichlorosilane, and 2.71 g (20.0 mmol) of trichlorosilane were reacted at 160° C. for 15 hrs. The resulting mixture was distilled to give 1.13 g of 1,1,1,3,3,3-hexachloro-1,3-disilapropane (yield; 68%). The resulting mixture was distilled

反応条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 2-L flask equipped with magnetic stirring, pot thermometer, addition funnel and condenser was charged with a mixture of 1455 g (2.05 mol) containing approximately 46% (dichlorosilylmethyl)trichlorosilane and 54% bis(trichlorosilyl)methane [molar ratio 1:1]. To the addition funnel were added 186 g (2.05 mol) of methallyl chloride. The reaction mixture was heated to 110° C. and 20 g of the olefin and 0.5 mL of a 5% solution of chloroplatinic acid in tetrahydrofuran were added to the reaction mixture to initiate the reaction. The remainder of the olefin was added to the reaction mixture at an appropriate rate to maintain the reaction temperature between 110 and 120° C. After completion of the olefin addition, the reaction mixture was heated to 130° C. for an additional 3 hours. Distillation of the product directly from the reaction mixture yielded 412 g (60%) of the title dipodal silane, bp 89-91° C./0.4 mm Hg, density @ 20° C. 1.380. A 2-L flask equipped with magnetic stirring pot thermometer, addition funnel and condenser was charged with a mixture of 1455 g (2.05 mol) the reaction to maintain the reaction temperature between 110 and 120° C the reaction mixture was heated to 130° C. for an additional 3 hours Distillation of the product directly from the reaction mixture

反応条件: temp:90.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under a nitrogen atmosphere a 1-liter, 3-necked flask equipped with a heating mantle, magnetic stirrer, pot thermometer, addition funnel and condenser was charged with 276.8 g of a mixture of approximately 46% (dichlorosilylmethyl)trichlorosilane and 54% bis(trichlorosilyl)methane [molar ratio 1:1]. The mixture was heated to 90° C. and 10 g of decene were added to the mixture via addition funnel, followed by 0.5 ml of 5% hexachloroplatinic acid in tetrahydrofuran. An immediate exotherm was observed and the reaction mixture changed from clear to dark brown. An additional 173 g of decene were added at an appropriate rate to maintain the temperature between 90 and 110° C. Upon completion of the addition, an additional 0.25 ml of 5% hexachloroplatinic acid solution was added and the mixture was stirred at 100° C. for 45 minutes. GC analysis of the mixture indicated the presence of some unreacted pentachlorodisilapropane. An additional 10 g of decene were added and the reaction mixture was stirred an additional 45 minutes at 100° C. Distillation provided 242 g (59%) of the title compound, bp 126° C./0.1 mm Hg, density @ 20° C. 1.180. Under a nitrogen atmosphere a 1-liter, 3-necked flask equipped with a heating mantle, magnetic stirrer pot thermometer, addition funnel and condenser to maintain the temperature between 90 and 110° C Upon completion of the addition the reaction mixture was stirred an additional 45 minutes at 100° C Distillation

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 procedure as Example 1 above, 0.20 g (0.75 mmol) of triphenylphosphine, 0.92 g (7.5 mmol) of (chloromethyl)trichlorosilane, and 5.08 g (37.5 mmol) of trichlorosilane were reacted at 150° C. for 42 hrs. The resulting mixture was distilled to give 1.1 g of 1,1,1,3,3,3-hexachloro-1,3-disilapropane (bp; 173-174° C., yield; 50%) and 0.3 g of 1,1,1,3,3-pentachloro-1,3-disilapropane (bp; 166-167° C., yield; 16%). The resulting mixture was distilled