3-trimethylsilylpropanoyl chloride

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 13.5 g (0.11 mol) of thionyl chloride are added dropwise with stirring to a mixture of 10 g (0.068 mol) of 3-trimethylsilylpropanoic acid in 30 ml of 1,2-dichloroethane. The reaction mixture is heated at 40° C. for 2 hours. The excess thionyl chloride is removed by distillation under reduced pressure. The solution obtained is used without further purification for the following step. The excess thionyl chloride is removed by distillation under reduced pressure The solution obtained is used without further purification for the following step

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 13.5 g (0.11 mol) of thionyl chloride are added dropwise with stirring to a mixture of 10 g (0.068 mol) of 3-trimethylsilylpropanoic acid in 30 ml of 1,2-di-chloroethane. The reaction mixture is heated at 40° C. for 2 hours. The excess thionyl chloride is removed by distillation under reduced pressure. The solution obtained is used without further purification for the following step. The excess thionyl chloride is removed by distillation under reduced pressure The solution obtained is used without further purification for the following step

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 13.5 g (0.11 mol) of thionyl chloride are added dropwise with stirring to a mixture of 10 g (0.068 mol) of 3-trimethylsilylpropanoic acid in 30 ml of 1,2-dichloroethane. The reaction mixture is heated at 40° C. for 2 hours. The excess thionyl chloride is removed by distillation under reduced pressure. The solution obtained is used without further purification for the following step. The excess thionyl chloride is removed by distillation under reduced pressure The solution obtained is used without further purification for the following step

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 13.5 g (0.11 mol) of thionyl chloride are added dropwise with stirring to a mixture of 10 g (0.068 mol) of 3-trimethylsilylpropanoic acid in 30 ml of 1,2-dichloroethane. The reaction mixture is heated at 40° C. for 2 hours. The excess thionyl chloride is removed by distillation under reduced pressure. The solution obtained is used without further purification for the following step. The excess thionyl chloride is removed by distillation under reduced pressure The solution obtained is used without further purification for the following step

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 13.5 g (0.11 mol) of thionyl chloride are added dropwise with stirring to a mixture of 10 g (0.068 mol) of 3-trimethylsilylpropanoic acid in 30 ml of 1,2-dichloroethane. The reaction mixture is heated at 40° C. for 2 hours. The excess thionyl chloride is removed by distillation under reduced pressure. The solution obtained is used without further purification for the following step. The excess thionyl chloride is removed by distillation under reduced pressure The solution obtained is used without further purification for the following step

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 13.5 g (0.11 mol) of thionyl chloride were added dropwise at room temperature to a solution of 10 g (0.068 mol) of 3-trimethylsilylpropionic acid in 50 ml of 1,2-dichloroethane. The mixture was heated at 40° C. for 2 hours, and the excess thionyl chloride was distilled under vacuum. A solution of 3-trimethylsilylpropionic acid chloride was obtained in 1,2-dichloroethane, which solution was used as is in the next step. the excess thionyl chloride was distilled under vacuum

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

実験手順: In a flask were placed 5.0 g (0.032 mole) of 4,4-dimethyl-4-silapentanoic acid chloride and 2.89 g (0.032 mole) of copper(I) cyanide. This mixture was heated at approximately 150°-200° C. for a period of 50 minutes after which it was cooled to ambient temperature. Methylene chloride was added to the reaction mixture which was then filtered. The solvent was evaporated from the filtrate under reduced pressure, leaving 1.5 g of 4,4-dimethyl-4-silapentanoyl cyanide as a residue. In a flask were placed This mixture was heated at approximately 150°-200° C. for a period of 50 minutes after which it was then filtered The solvent was evaporated from the filtrate under reduced pressure

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

実験手順: In a flask were place 13.4 g (0.0918 mole) of 4,4-dimethyl-4-silapentanoic acid, 100 mL of diethyl ether, and two drops of N,N-dimethylformamide. To this solution, which was cooled in an ice/water bath, was added 13.98 g (0.110 mole) of oxalyl chloride in diethyl ether in a dropwise manner. Upon completion of addition, the temperature was allowed to rise to ambient conditions, and the mixture was stirred for approximately 16 hours. At the conclusion of this period the solvent was evaporated from the reaction mixture under reduced pressure, leaving 10.42 g of 4,4-dimethyl-4-silapentanoic acid chloride as a residue. The NMR spectrum was consistent with the proposed structure. In a flask were To this solution, which was cooled in an ice/water bath Upon completion of addition At the conclusion of this period the solvent was evaporated from the reaction mixture under reduced pressure

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 13.5 g (0.11 mol) of thionyl chloride are added dropwise with stirring to a mixture of 10 g (0.068 mol) of 3-trimethylsilylpropanoic acid in 30 ml of 1,2-di-chloroethane. The reaction mixture is heated at 40° C. for 2 hours. The excess thionyl chloride is removed by distillation under reduced pressure. The solution obtained is used without further purification for the following step. The excess thionyl chloride is removed by distillation under reduced pressure The solution obtained is used without further purification for the following step

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 13.5 g (0.11 mol) of thionyl chloride are added dropwise with stirring to a mixture of 10 g (0.068 mol) of 3-trimethylsilylpropanoic acid in 30 ml of 1,2-dichloroethane. The reaction mixture is heated at 40° C. for 2 hours. The excess thionyl chloride is removed by distillation under reduced pressure. The solution obtained is used without further purification for the following step. The excess thionyl chloride is removed by distillation under reduced pressure The solution obtained is used without further purification for the following step

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 13.5 g (0.11 mol) of thionyl chloride are added dropwise with stirring to a mixture of 10 g (0.068 mol) of 3-trimethylsilylpropanoic acid in 30 ml of 1,2-dichloroethane. The reaction mixture is heated at 40° C. for 2 hours. The excess thionyl chloride is removed by distillation under reduced pressure. The solution obtained is used without further purification for the following step. The excess thionyl chloride is removed by distillation under reduced pressure The solution obtained is used without further purification for the following step