HRID2209690

反应详情

EQUATION

反应方程式

HRID 2209690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[N-t-Butyloxycarbamoyl]-4-[[4-methoxybenzenesulfonyl](benzyl)amino]-1-[benzyl]-piperidine is dissolved in dichloroethane (60 mL) and ethanol (1.0 mL) in a glass sealed tube. Hydrochloric acid gas (from a lecture bottle) is bubbled through the solution for 30 minutes at -10° C. The tube is sealed, gradually warmed to room temperature, and stirred overnight. At this point, hydrochloric acid gas is again bubbled through the reaction mixture as done previously and stirred at room temperature for an additional 24 hours. The reaction mixture is reduced to 1/3 volume in vacuo and triturated with diethyl ether. The solid is filtered off and dried in vacuo to provide 4-[N-hydroxy-carbamoyl]-4-[[4-methoxybenzenesulfonyl](benzyl)amino]-1-[benzyl]-piperidine, m.p. 135.5°-142° C.

WORKUP

后处理

  1. customHydrochloric acid gas (from a lecture bottle) is bubbled through the solution for 30 minutes at -10° C
  2. customThe tube is sealed
  3. customAt this point, hydrochloric acid gas is again bubbled through the reaction mixture
  4. stirringstirred at room temperature for an additional 24 hours
  5. customtriturated with diethyl ether
  6. filtrationThe solid is filtered off
  7. customdried in vacuo