反应详情

HCl is passed into a suspension of 10 g of finely powdered 1-benzyl-4-amino-4-piperidinecarboxylic acid in 111 ml of CH2Cl2 at 0° C. for 1 hour. 26 g of PCl5 in 200 ml of CH2Cl2 are added in several portions to this mixture, with vigorous stirring and while passing in further HCl. After the mixture has been stirred at 0° C. for 4 hours, the reaction product is filtered off with suction over a glass frit, with exclusion of moisture, and washed thoroughly with petroleum ether (60°-80° C.) and CH2Cl2. The crude product thus obtained is used in the next reaction stage without further purification.

1. stirringAfter the mixture has been stirred at 0° C. for 4 hours
2. filtrationthe reaction product is filtered off with suction over a glass frit, with exclusion of moisture
3. washwashed thoroughly with petroleum ether (60°-80° C.) and CH2Cl2