HRID1463034

反应详情

EQUATION

反应方程式

HRID 1463034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (S)-1,4-dithia-7-azaspiro[4.4]nonane-8-carboxylic acid, p-toluenesulfonate (6.0 g.) in 30 ml. of anhydrous dimethylformamide at 50 ° under argon is added a dimethylformamide solution of diphenyldiazomethane (3.6) portionwise. After 10 minutes at 50°, the solvent is removed under reduced pressure. The residue is dissolved in ethyl acetate and precipitated with ether. The solvent is then decanted and the residue triturated with ethyl acetate/ether to give (S)-1,4-dithia-7-azaspiro [4.4]nonane-8-carboxylic acid, diphenylmethyl ester, p-toluenesulfonate.

WORKUP

后处理

  1. customthe solvent is removed under reduced pressure
  2. dissolutionThe residue is dissolved in ethyl acetate
  3. customprecipitated with ether
  4. customThe solvent is then decanted
  5. customthe residue triturated with ethyl acetate/ether