HRID854259

反应详情

EQUATION

反应方程式

HRID 854259 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

279 mg of 4-(4-chloro-2-methyl-pyrrolo[2,3-d]pyrimidin-7-yl)-butyric acid ethyl ester (example 2a) and 655 mg of N-(4-bromobenzenesulfonyl)-(R)-cysteine-tert-butyl ester (example 6b) were dissolved in 2 ml of NMP and 0.68 ml of DIPEA were added. The reaction mixture was heated to 100° C. for 4 h. The mixture was diluted with 60 ml of EE and extracted with 10% citric acid, saturated NaCl solution and with water. The organic phase was dried over MgSO4 and the solvent was removed in vacuo. The crude product was chromatographed on silica gel eluting with EE/toluene (1:6). Yield: 108 mg.

WORKUP

后处理

  1. additionThe mixture was diluted with 60 ml of EE
  2. extractionextracted with 10% citric acid, saturated NaCl solution and with water
  3. dry with materialThe organic phase was dried over MgSO4
  4. customthe solvent was removed in vacuo
  5. customThe crude product was chromatographed on silica gel eluting with EE/toluene (1:6)