HRID72240

反应详情

EQUATION

反应方程式

HRID 72240 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 3-[4-(3-Dimethylamino-pyrrolidin-1-yl)-phenyl]-6-hydroxymethyl-3H-thieno[3,2-d]pyrimidin-4-one (50.0 mg), sodium hydride (5.24 mg) and DMF (1 mL) was stirred at 0° C. for 15 min. Then 1-bromopropane (22.0 mg) was added, the solution was warmed to room temperature and stirred for 2 h. Water and ethyl acetate were added and the aqueous phase was extracted with ethyl acetate several times. The combined organic phase was dried over sodium sulfate and the solvent removed in vacuo. The crude product was purified by preparative HPLC. The product with the molecular weight of 412.55 (C22H28N4O2S) was obtained in this way; MS (ESI): 413 (M+H+).

WORKUP

后处理

  1. temperaturethe solution was warmed to room temperature
  2. stirringstirred for 2 h
  3. extractionthe aqueous phase was extracted with ethyl acetate several times
  4. dry with materialThe combined organic phase was dried over sodium sulfate
  5. customthe solvent removed in vacuo
  6. customThe crude product was purified by preparative HPLC
  7. customThe product with the molecular weight of 412.55 (C22H28N4O2S) was obtained in this way