1,1-二氯硅杂环己烷

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a flask containing 100 ml of tetrahydrofuran, 2,3,4,5-tetramethylcyclopenta-2,4-diene (3.67 g, 30 mmol) was added, and then n-butyl lithium (12 ml) was added in droplets thereto at 0° C. The reaction temperature was gradually increased to room temperature, and the reaction mixture was allowed to react for 8 hours. The temperature of the reaction solution was decreased to −78° C., after which the reaction solution was added with dichlorosilacyclohexane (5.07 g, 30 mmol) and then allowed to react for 12 hours. After the reaction, volatile material was removed, the resultant reaction product was extracted with 100 ml of hexane, and more volatile material was removed, thus obtaining 7.01 g of chloro-2,3,4,5-tetramethylcyclopentadienyl silacyclohexane as light yellow oil. Subsequently, the chloro-2,3,4,5-tetramethylcyclopentadienyl silacyclohexane thus obtained was dissolved in 100 ml of tetrahydrofuran, without additional purification, and 2.18 g of lithium tert-butylamide was added in droplets thereto at 0° C., after which the reaction mixture was allowed to react at room temperature for 2 hours. After the reaction, the volatile material was removed, the resultant reaction product was extracted with 100 ml of hexane, and more volatile material was removed, thus obtaining 7.42 g of (tert-butylamido)(2,3,4,5-tetramethylcyclopenta-2,4-dienyl)silacyclohexane as light yellow oil. was added at 0° C to react for 8 hours was decreased to −78° C. to react for 12 hours After the reaction, volatile material was removed the resultant reaction product was extracted with 100 ml of hexane, and more volatile material was removed

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of cyclopentamethylenedichlorosilane (0.5 mL; 3.42 mmol) in dry THF (10 mL) was added urea (0.246 g; 4.10 mmol). The mixture was then cooled to 0° C. and benzyl glycolate (0.48 mL; 3.42 mmol) was added dropwise over a 15 minute span. The mixture was then taken off the ice bath and allowed to stir at room temperature for 40 minutes. The mixture was then concentrated under high vacuum and diluted with chloroform. The aqueous layer was soaked up with excess Na2SO4 and the mixture was filtered. The filtrate was concentrated to a light yellow crude liquid which was used without further purification. The mixture was then concentrated under high vacuum diluted with chloroform the mixture was filtered The filtrate was concentrated to a light yellow crude liquid which was used without further purification

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Into a flask containing 100 ml of tetrahydrofuran, 2,3,4,5-tetramethylcyclopenta-2,4-diene (3.67 g, 30 mmol) was added, and then n-butyl lithium (12 ml) was added in droplets thereto at 0° C. The reaction temperature was gradually increased to room temperature, and the reaction mixture was allowed to react for 8 hours. The temperature of the reaction solution was decreased to −78° C., after which the reaction solution was added with dichlorosilacyclohexane (5.07 g, 30 mmol) and then allowed to react for 12 hours. After the reaction, volatile material was removed, the resultant reaction product was extracted with 100 ml of hexane, and more volatile material was removed, thus obtaining 7.01 g of chloro-2,3,4,5-tetramethylcyclopentadienyl silacyclohexane as light yellow oil. Subsequently, the chloro-2,3,4,5-tetramethylcyclopentadienyl silacyclohexane thus obtained was dissolved in 100 ml of tetrahydrofuran, without additional purification, and 2.18 g of lithium tert-butylamide was added in droplets thereto at 0° C., after which the reaction mixture was allowed to react at room temperature for 2 hours. After the reaction, the volatile material was removed, the resultant reaction product was extracted with 100 ml of hexane, and more volatile material was removed, thus obtaining 7.42 g of (tert-butylamido)(2,3,4,5-tetramethylcyclopenta-2,4-dienyl)silacyclohexane as light yellow oil. was added at 0° C to react for 8 hours was decreased to −78° C. to react for 12 hours After the reaction, volatile material was removed the resultant reaction product was extracted with 100 ml of hexane, and more volatile material was removed

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of cyclopentamethylenedichlorosilane (0.5 mL; 3.42 mmol) in dry THF (10 mL) was added urea (0.246 g; 4.10 mmol). The mixture was then cooled to 0° C. and benzyl glycolate (0.48 mL; 3.42 mmol) was added dropwise over a 15 minute span. The mixture was then taken off the ice bath and allowed to stir at room temperature for 40 minutes. The mixture was then concentrated under high vacuum and diluted with chloroform. The aqueous layer was soaked up with excess Na2SO4 and the mixture was filtered. The filtrate was concentrated to a light yellow crude liquid which was used without further purification. The mixture was then concentrated under high vacuum diluted with chloroform the mixture was filtered The filtrate was concentrated to a light yellow crude liquid which was used without further purification