HRID2049995

反应详情

EQUATION

反应方程式

HRID 2049995 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 500 mg (3.26 mmoles) of 3-hydroxyazetidine-3-carboxylic acid hydrochloride in 15 ml of water are added 1.06 ml of 37% formalin and 250 mg of platinum oxide monohydrate, and the mixture is kept at ambient temperature under atmospheric pressure for 46 hours. The catalyst is filtered off and washed with water. The combined filtrate and washings are evaporated under reduced pressure. The residue (0.79 g) is dissolved in 10 ml of water, adsorbed on 30 ml of Amberlite IR-120 B (H+), and eluted with 100 ml of 2 N aqueous ammonium hydroxide solution. The eluate is evaporated under reduced pressure. The residue (431 mg) is crystallized from water-acetone to yield 1-methyl-3-hydroxyazetidine-3-carboxylic acid as prisms.

WORKUP

后处理

  1. filtrationThe catalyst is filtered off
  2. washwashed with water
  3. customThe combined filtrate and washings are evaporated under reduced pressure
  4. dissolutionThe residue (0.79 g) is dissolved in 10 ml of water
  5. washeluted with 100 ml of 2 N aqueous ammonium hydroxide solution
  6. customThe eluate is evaporated under reduced pressure
  7. customThe residue (431 mg) is crystallized from water-acetone