trichloro(3,3,3-trifluoropropyl)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:; See reaction.notes.procedure_details.

実験手順: In the same apparatus and procedure as Example 1 above, 0.15 g (0.75 mmol) of tri-n-butylphosphine, 1.33 g (10.0 mmol) of 1-chloro-3,3,3-trifluoropropane, and 6.77 g (50.0 mmol) of trichlorosilane were reacted at 150° C. for 15 hrs. The resulting mixture was distilled to give 2.1 g of (3,3,3-trifluoropropyl)trichlorosilane (bp; 114° C., yield; 90%). The resulting mixture was distilled

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:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2 moles CF3CH2CH2SiCl3, 3.5 moles Me2SiHCl, and 2.6 moles tetra(n-butyl)ammonium chloride were introduced into a flask and heated under reflux for 3 days with stirring. A mixture of chlorosilanes was then recovered by distillation in vacuo. According to analysis by gas chromatography, the main components of the reaction product were CF3CH2CH2SiCl3, CF3CH2CH2SiHCl2, Me2SiHCl, and Me2SiCl2. The CF3CH2CH2SiCl3 and CF3CH2CH2SiHCl2 fraction was isolated by distillation in vacuo. The CF3CH2CH2SiCl3 and CF3CH2CH2SiHCl2 mixture was placed in a flask, 5 g isopropanolic chloroplatinic acid solution (concentration=10%) was added, and, while stirring and heating to 50° C., CF3CH=CH2 gas was then continuously injected through a glass tube inserted into the liquid. Its addition was halted when the peak for CF3CH2CH2SiHCl2 had disappeared in gas chromoatographic analysis. (CF3CH2CH2)2SiCl2 (bp=128° C./20 mmHg) was then isolated by distillation in vacuo. CF3CH=CH2 gas was then continuously injected through a glass tube Its addition

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

実験手順: 2 moles CF3CH2CH2SiCl3, 3.5 moles Me2SiHCl, and 2.6 moles tetra(n-butyl)ammonium chloride were introduced into a flask and heated under reflux for 3 days with stirring. A mixture of chlorosilanes was then recovered by distillation in vacuo. According to analysis by gas chromatography, the main components of the reaction product were CF3CH2CH2SiCl3, CF3CH2CH2SiHCl2, Me2SiHCl, and Me2SiCl2. The CF3CH2CH2SiCl3 and CF3CH2CH2SiHCl2 fraction was isolated by distillation in vacuo. The CF3CH2CH2SiCl3 and CF3CH2CH2SiHCl2 mixture was placed in a flask, 5 g isopropanolic chloroplatinic acid solution (concentration=10%) was added, and, while stirring and heating to 50° C., CF3CH=CH2 gas was then continuously injected through a glass tube inserted into the liquid. Its addition was halted when the peak for CF3CH2CH2SiHCl2 had disappeared in gas chromoatographic analysis. (CF3CH2CH2)2SiCl2 (bp=128° C./20 mmHg) was then isolated by distillation in vacuo. heated under reflux for 3 days was then recovered by distillation in vacuo

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

実験手順: 2 moles CF3CH2CH2SiCl3, 3.5 moles Me2SiHCl, and 2.6 moles tetra(n-butyl)ammonium chloride were introduced into a flask and heated under reflux for 3 days with stirring. A mixture of chlorosilanes was then recovered by distillation in vacuo. According to analysis by gas chromatography, the main components of the reaction product were CF3CH2CH2SiCl3, CF3CH2CH2SiHCl2, Me2SiHCl, and Me2SiCl2. The CF3CH2CH2SiCl3 and CF3CH2CH2SiHCl2 fraction was isolated by distillation in vacuo. The CF3CH2CH2SiCl3 and CF3CH2CH2SiHCl2 mixture was placed in a flask, 5 g isopropanolic chloroplatinic acid solution (concentration=10%) was added, and, while stirring and heating to 50° C., CF3CH=CH2 gas was then continuously injected through a glass tube inserted into the liquid. Its addition was halted when the peak for CF3CH2CH2SiHCl2 had disappeared in gas chromoatographic analysis. (CF3CH2CH2)2SiCl2 (bp=128° C./20 mmHg) was then isolated by distillation in vacuo. heated under reflux for 3 days was then recovered by distillation in vacuo

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 (0.68 mmol) of tetrabutylphosphonium chloride, 0.89 g (6.72 mmol) of 1-chloro-3,3,3-trifluoropropane, and 2.71 g (20.0 mmol) of trichlorosilane were reacted at 150° C. for 10 hrs. The resulting mixture was distilled to give 1.24 g of (3,3,3-trifluoropropyl)trichlorosilane (yield; 80%). The resulting mixture was distilled

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

実験手順: In an oven-dried 250-mL round bottom flask, 4.12 g (42.0 mmol) of trimethylsilylacetylene was dissolved in 45 mL of anhydrous THF. The solution was cooled to 0° C., then n-butyllithium (14.8 mL, 37 mmol, 2.5 M in hexane) was added dropwise. Stirring was continued for 1 hr and the colorless solution was allowed to warm to room temperature. In a second oven-dried 500-mL round bottom flask, 3,3,3-trifluoropropyltrichlorosilane (8.1 g, 35 mmol) was dissolved in anhydrous THF (35 mL). The first reaction mixture was added to the second solution dropwise over 1 hr, followed by stirring for 5 hrs. The new reaction mixture was cooled to 0° C., then isopropyllithium (123 mL, 86 mmol, 0.7 M in pentane) was added dropwise, and the solution was allowed to warm to room temperature over 12 hrs. The entire mixture was poured into 150 mL of a dilute solution of ammonium chloride, and hexane (100 mL) was added. The organic layer was separated, and the aqueous layer was extracted a second time with hexane (20 mL). The organic layers were combined, washed with water (3×20 mL), dried over magnesium sulfate, filtered, and concentrated under vacuum. The trimethylsilyl-capped product was purified by column chromatography on silica gel using hexane as an eluant (Rf˜0.6 in hexane), yielding 7.7 g of a colorless liquid. The trimethylsilyl group was removed by dissolving the product in THF (20 mL) and adding methanol (20 mL) and 3 drops of a 15% sodium hydroxide solution, followed by stirring for 30 minutes. The crude product was isolated, then flushed through a thin pad of silica using hexane and concentrated under vacuum to yield 4.9 g (21 mmol, 60% from the starting silane) of a colorless liquid. Analysis of the colorless product provided the following data: 1H-NMR (200 MHz, CDCl3) δ=2.4 (s, 1H), 2.2 (m, 2H), 1.1 (m, 14H), 0.8 (m, 2H). to warm to room temperature In a second oven-dried 500-mL round bottom flask The first reaction mixture was added to the second solution dropwise over 1 hr by stirring for 5 hrs The new reaction mixture was cooled to 0° C. to warm to room temperature over 12 hrs was added The organic layer was separated the aqueous layer was extracted a second time with hexane (20 mL) washed with water (3×20 mL) dried over magnesium sulfate filtered concentrated under vacuum The trimethylsilyl-capped product was purified by column chromatography on silica gel

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, 0.15 g (0.75 mmol) of tri-n-butylphosphine, 1.33 g (10.0 mmol) of 1-chloro-3,3,3-trifluoropropane, and 6.77 g (50.0 mmol) of trichlorosilane were reacted at 150° C. for 15 hrs. The resulting mixture was distilled to give 2.1 g of (3,3,3-trifluoropropyl)trichlorosilane (bp; 114° C., yield; 90%). The resulting mixture was distilled