HRID58267

反应详情

EQUATION

反应方程式

HRID 58267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of 7-(1-bromo ethyl)-5H-[1,3]thiazolo[3,2-a]pyrimidin-5-one (17.5 g, 67.5 mmol) and N-bromosuccinimide (14.2 g, 79.8 mmol) in acetonitrile (400 mL) was stirred at 80° C. under N2 overnight. After removal of the solvent under reduced pressure, the resulting solid was dissolved in dichloromethane, washed sequentially with water, saturated aqueous Na2S2O3 and NaHCO3 solution and brine, dried over Na2SO4, and then concentrated to give crude product (3.7 g), which was used in the next step without further purification. LCMS calculated for C8H7Br2N2OS (M+H)+: m/z=336.9. Found: 336.9.

WORKUP

后处理

  1. customAfter removal of the solvent under reduced pressure
  2. dissolutionthe resulting solid was dissolved in dichloromethane
  3. washwashed sequentially with water, saturated aqueous Na2S2O3 and NaHCO3 solution and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated