HRID1013338

反应详情

EQUATION

反应方程式

HRID 1013338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 3-phenyl-1-oxa-2-azaspiro[4.5]dec-2-ene-8-carboxylic acid ethyl ester (190 mg, 0.67 mmol) in MeOH (5 ml) and lithium hydroxide monohydrate (74 mg, 1.0 mmol) in H2O (1 ml) was stirred overnight at RT. After removal of the solvent under vacuum, the residue was taken up in 10% aq. citric acid solution and EtOAc and the phases were separated. The aqueous phase was extracted several times with EtOAc, dried over magnesium sulphate and desolventised under vacuum. 150 g (87% of the theoretical amount) of the free acid 3-phenyl-1-oxa-2-azaspiro[4.5]dec-2-ene-8-carboxylic acid was obtained in the form of a colourless solid.

WORKUP

后处理

  1. customAfter removal of the solvent under vacuum
  2. customEtOAc and the phases were separated
  3. extractionThe aqueous phase was extracted several times with EtOAc
  4. dry with materialdried over magnesium sulphate