HRID1634204

反应详情

EQUATION

反应方程式

HRID 1634204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Phenyl-4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridine (0.11 g) was added to a solution of 2-chlorosulfonylmethyl-3-methyl-butyric acid tert-butyl ester (0.14 g) and triethylamine (0.3 ml) in DCM (20 ml) at room temperature. The solution was stirred for 2 h, then TFA (5 ml) was added and the mixture stirred for 1 h. The mixture was evaporated in vacuo and the residue partitioned between diethyl ether (10 ml) and saturated sodium bicarbonate (30 ml). The aqueous layer was acidified with citric acid to pH 5 and extracted with ethyl acetate (3×20 ml). The solvent was dried (MgSO4) and evaporated to give the title compound as pale yellow solid (0.15 g).

WORKUP

后处理

  1. stirringthe mixture stirred for 1 h
  2. customThe mixture was evaporated in vacuo
  3. customthe residue partitioned between diethyl ether (10 ml) and saturated sodium bicarbonate (30 ml)
  4. extractionextracted with ethyl acetate (3×20 ml)
  5. dry with materialThe solvent was dried (MgSO4)
  6. customevaporated