trichloro(3-chloropropyl)silane

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In Step 1, a halogenated silane, such as 3-chloropropyldimethylchlorosilane, is reacted with a Grinard reagent, such as vinyl magnesium chloride, to form 3-chloropropyldimethylvinylsilane. When 3-chloropropylmethyldichlorosilane or 3-chloropropyltrichlorosilane is used as the halogenated silane instead of 3-chloropropyldimethylchlorosilane, 3-chloropropylmethyldivinylsilane or 3-chloropropyltrivinylsilane is obtained, respectively. The reaction is generally carried out by dropwise adding the halogenated silane to a solution of vinyl magnesium chloride in THF. The reaction temperature may be in a range of from 20 to 75 degrees C. The reaction is exothermic. Therefore, if the temperature rises too high, the reaction mixture may be cooled. After the completion of the addition, the reaction mixture is stirred for further 30 minutes to 10 hours. Then, the salt is dissolved in diluted hydrochloric acid and the organic phase is recovered and purified to obtain an intermediate product.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In the same apparatus and procedure as Example 1 above, 0.037 g (0.14 mmol) of triphenylphosphine, 1.07 g (14.0 mmol) of allyl chloride, and 9.48 g (70.0 mmol) of trichlorosilane were reacted at 150° C. for 10 hrs. The resulting mixture was distilled to give 1.2 g of allytrichlorosilane (bp; 117-8° C., yield; 49%), 0.12 g of propyltrichlorosilane (bp; 123-5° C., yield; 5%), and 0.24 g of (3-chloropropyl)trichlorosilane (bp; 181-2° C., yield; 8%). The resulting mixture was distilled

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In the same apparatus and procedure as Example 1 above, 0.037 g (0.14 mmol) of triphenylphosphine, 1.07 g (14.0 mmol) of allyl chloride, and 9.48 g (70.0 mmol) of trichlorosilane were reacted at 150° C. for 10 hrs. The resulting mixture was distilled to give 1.2 g of allytrichlorosilane (bp; 117-8° C., yield; 49%), 0.12 g of propyltrichlorosilane (bp; 123-5° C., yield; 5%), and 0.24 g of (3-chloropropyl)trichlorosilane (bp; 181-2° C., yield; 8%). The resulting mixture was distilled

Conditions: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 15.306 grams of allyl chloride, 27.09 gram of trichlorosilane and 0.04 grams of [SG]--S--Pt sufficient to provide 1×10-5 mm Pt/SiH was stirred at 23° C. under a nitrogen atmosphere. The mixture was heated to 60° C. for 16 hours. The mixture was allowed to cool to ambient temperatures and was diluted with 50 ml of hexane and filtered. The filtrate was concentrated on a rotary evaporator to give 33 grams of a clear, colorless oil. Based on method of preparation, NMR and VPC analysis there was obtained about a 92% yield of γ-chloropropyltrichlorosilane and about an 8% yield of n-propyltrichlorosilane. to provide 1×10-5 mm Pt/SiH The mixture was heated to 60° C. for 16 hours to cool to ambient temperatures filtered The filtrate was concentrated on a rotary evaporator to give 33 grams of a clear, colorless oil Based on method of preparation, NMR

Conditions: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 15.306 grams of allyl chloride, 27.09 gram of trichlorosilane and 0.04 grams of [SG]--S--Pt sufficient to provide 1×10-5 mm Pt/SiH was stirred at 23° C. under a nitrogen atmosphere. The mixture was heated to 60° C. for 16 hours. The mixture was allowed to cool to ambient temperatures and was diluted with 50 ml of hexane and filtered. The filtrate was concentrated on a rotary evaporator to give 33 grams of a clear, colorless oil. Based on method of preparation, NMR and VPC analysis there was obtained about a 92% yield of γ-chloropropyltrichlorosilane and about an 8% yield of n-propyltrichlorosilane. to provide 1×10-5 mm Pt/SiH The mixture was heated to 60° C. for 16 hours to cool to ambient temperatures filtered The filtrate was concentrated on a rotary evaporator to give 33 grams of a clear, colorless oil Based on method of preparation, NMR

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Gamma-chloropropyltrichlorosilane (21.2 g., 0.1 mole) is dissolved in 200 ml. of dry ether and an ether slurry of (33.6g, 0.3 mole) sodium trimethylsilanoate, (CH3)3SiONa, is added in small portions. The mixture is allowed to stand for 12 hours and is then refluxed for an additional 3 hours. Filtration of the sodium chloride and removal of the ether from the filtrate leaves gamma-chloropropyltris-trimethylsiloxysilane. is then refluxed for an additional 3 hours Filtration of the sodium chloride and removal of the ether from the filtrate

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Gamma-chloropropyltrichlorosilane (21.2 g., 0.1 mole) is dissolved in 200 ml. of dry ether and an ether slurry of (33.6g, 0.3 mole) sodium trimethylsilanoate, (CH3)3SiONa, is added in small portions. The mixture is allowed to stand for 12 hours and is then refluxed for an additional 3 hours. Filtration of the sodium chloride and removal of the ether from the filtrate leaves gamma-chloropropyltris-trimethylsiloxysilane. is then refluxed for an additional 3 hours Filtration of the sodium chloride and removal of the ether from the filtrate

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In a 100 ml apparatus, there were combined 7.1 g (0.075 mol) of Me2SiHCl, 10.2 g (0.075 mol) of Cl3SiH, and 5.7 g (0.075 mol) of allyl chloride. Pt catalyst solution (0.01 ml) was added at 33° C., causing an exothermic reaction to 47° C. in 7 min. VPC analysis 14 min. later showed a complete reaction. Vacuum distillation yielded 60.4% Cl3SiCH2CH2CH2Cl and 8.6% Me2SiClCH2CH2CH2Cl. This example shows that Me2SiHCl is an effective promoter for the reaction of Cl3SiH with allyl chloride at the equimolar level. an exothermic reaction to 47° C. in 7 min VPC analysis 14 min. a complete reaction Vacuum distillation

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In a 100 ml apparatus, there were combined 7.1 g (0.075 mol) of Me2SiHCl, 10.2 g (0.075 mol) of Cl3SiH, and 5.7 g (0.075 mol) of allyl chloride. Pt catalyst solution (0.01 ml) was added at 33° C., causing an exothermic reaction to 47° C. in 7 min. VPC analysis 14 min. later showed a complete reaction. Vacuum distillation yielded 60.4% Cl3SiCH2CH2CH2Cl and 8.6% Me2SiClCH2CH2CH2Cl. This example shows that Me2SiHCl is an effective promoter for the reaction of Cl3SiH with allyl chloride at the equimolar level. an exothermic reaction to 47° C. in 7 min VPC analysis 14 min. a complete reaction Vacuum distillation

Conditions: temp:23.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 15.306 grams of allyl chloride, 27.09 gram of trichlorosilane and 0.04 grams of [SG]--S--Pt sufficient to provide 1×10-5 mm Pt/SiH was stirred at 23° C. under a nitrogen atmosphere. The mixture was heated to 60° C. for 16 hours. The mixture was allowed to cool to ambient temperatures and was diluted with 50 ml of hexane and filtered. The filtrate was concentrated on a rotary evaporator to give 33 grams of a clear, colorless oil. Based on method of preparation, NMR and VPC analysis there was obtained about a 92% yield of γ-chloropropyltrichlorosilane and about an 8% yield of n-propyltrichlorosilane. to provide 1×10-5 mm Pt/SiH The mixture was heated to 60° C. for 16 hours to cool to ambient temperatures filtered The filtrate was concentrated on a rotary evaporator to give 33 grams of a clear, colorless oil Based on method of preparation, NMR

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In the same apparatus and procedure as Example 1 above, 0.44 g (1.50 mmol) of tetrabutylphosphonium chloride, 0.85 g (7.5 mmol) of 1,3-dichloropropane, and 10.16 g (75.0 mmol) of trichlorosilane were reacted at 150° C. for 10 hrs. The resulting mixture was distilled to give 1.68 g of 1,3-bis(trichlorosilyl)propane (yield; 72%) and 0.22 g of (3-chloropropyl)trichlorosilane (yield; 14%). The resulting mixture was distilled

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: In Step 1, a halogenated silane, such as 3-chloropropyldimethylchlorosilane, is reacted with a Grinard reagent, such as vinyl magnesium chloride, to form 3-chloropropyldimethylvinylsilane. When 3-chloropropylmethyldichlorosilane or 3-chloropropyltrichlorosilane is used as the halogenated silane instead of 3-chloropropyldimethylchlorosilane, 3-chloropropylmethyldivinylsilane or 3-chloropropyltrivinylsilane is obtained, respectively. The reaction is generally carried out by dropwise adding the halogenated silane to a solution of vinyl magnesium chloride in THF. The reaction temperature may be in a range of from 20 to 75 degrees C. The reaction is exothermic. Therefore, if the temperature rises too high, the reaction mixture may be cooled. After the completion of the addition, the reaction mixture is stirred for further 30 minutes to 10 hours. Then, the salt is dissolved in diluted hydrochloric acid and the organic phase is recovered and purified to obtain an intermediate product.