HRID399793

反应详情

EQUATION

反应方程式

HRID 399793 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 4-chloro-3-methylsulfonyl-5-nitrobenzoic acid (5.0 g) and piperidine (25.0 ml) was stirred for 1 hour at ambient temperature. To the mixture was added a mixture of ethyl acetate and water and the mixture was adjusted to pH 1 with conc. hydrochloric acid. The separated organic layer was washed with water and dried over magnesium sulfate. The solvent was removed by concentration and the residue was triturated with a mixture of diisopropyl ether and n-hexane to give 3-methylsulfonyl-5-nitro-4-piperidinobenzoic acid (5.66 g).

WORKUP

后处理

  1. additionTo the mixture was added
  2. washThe separated organic layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed by concentration
  5. customthe residue was triturated with a mixture of diisopropyl ether and n-hexane