HRID861337

反应详情

EQUATION

反应方程式

HRID 861337 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To L-penicillamine (15.75 g; 105.8 mmol) was added a solution of KOH (12.4 g; 222.2 mmol) in water (250 ml). When the solution was complete, Et2O (100 ml) was added and the solution cooled to 0° C. Benzyl chloroformate (14.9 ml; 105.8 mmol) was added dropwise and the stirred reaction mixture allowed to warm to RT. The layers were separated, the aqueous layer acidified to pH 1-1.5 with 1N hydrochloric acid, extracted with CH2Cl2 (×3) and dried (MgSO4). The solvent was removed in vacuo to yield N-benzyloxycarbonyl-L-penicillamine (21.27 g).

WORKUP

后处理

  1. customthe stirred reaction mixture
  2. temperatureto warm to RT
  3. customThe layers were separated
  4. extractionextracted with CH2Cl2 (×3)
  5. dry with materialdried (MgSO4)
  6. customThe solvent was removed in vacuo