HRID1755108

反应详情

EQUATION

反应方程式

HRID 1755108 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 6 M aqueous hydrochloric acid solution (217.9 ml, 1307.4 mmol) was slowly added to a suspension of 4-[2-(1,4-dioxa-8-aza-spiro[4.5]decane-8-sulfonyl)-ethyl]-3-methyl-benzoic acid (16.1 g, 43.58 mmol) in acetone (485 ml) at 0° C., and the mixture was warmed to room temperature and stirred overnight. The reaction mixture was filtered off, and the filtrate was then concentrated under reduced pressure. The precipitated solid was filtered off again. The solids filtered off were combined and dried to give 3-methyl-4-[2-(4-oxo-piperidine-1-sulfonyl)-ethyl]-benzoicacid as a white solid (13.62 g, 91.8%).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered off
  2. concentrationthe filtrate was then concentrated under reduced pressure
  3. filtrationThe precipitated solid was filtered off again
  4. filtrationThe solids filtered off
  5. customdried