HRID1981888

反应详情

EQUATION

反应方程式

HRID 1981888 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-t-Butoxycarbonyl-S-(2-aminoethyl)-L-cysteine (5.0 g) and N-hydroxysuccinimide (2.6 g) are dissolved in 500 ml of DMF. With cooling in an ice-bath, a solution of dicyclohexylcarbodiimide (4.7 g) in 10 ml of DMF is added dropwise over a period of 15 minutes. The reaction mixture is kept in a 4° room for 10 days. The solvent is then removed by lyophilization. The crude product is extracted into chloroform. Repeated chromatography on silica gel (20:1 chloroform-methanol) affords the pure product (3.1 g). The NMR spectrum is consistent with the assigned structure. A pure sample is obtained by recrystallization (ether-methanol) and analyzes for C10H18N2O3S.

WORKUP

后处理

  1. temperatureWith cooling in an ice-bath
  2. customis kept in a 4°
  3. customfor 10 days
  4. customThe solvent is then removed by lyophilization
  5. extractionThe crude product is extracted into chloroform