HRID232043

反应详情

EQUATION

反应方程式

HRID 232043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 20.5 g (72 mmol) of (R)-3-[(methylsulfonyl)oxy]-1-pyrrolidinecarboxylic acid, phenylmethyl ester in 100 ml of dry N,N-dimethylformamide was treated with 6.5 g (0.1 mol) of sodium azide and heated at 90° for four hours. The solvent was removed in high vacuo at 50° and the residue was partitioned between ethyl acetate/water (250 ml each). The aqueous layer was reextracted with ethyl acetate and the combined organic fractions were washed with water, dried (MgSO4) and evaporated in vacuo to give 16.2 g of the title compound.

WORKUP

后处理

  1. temperatureheated at 90° for four hours
  2. customThe solvent was removed in high vacuo at 50°
  3. customthe residue was partitioned between ethyl acetate/water (250 ml each)
  4. washthe combined organic fractions were washed with water
  5. dry with materialdried (MgSO4)
  6. customevaporated in vacuo