HRID2060252

反应详情

EQUATION

反应方程式

HRID 2060252 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 2-(4-chloro-phenyl)-5-methoxy-pyrimidine (100 mg, 0.45 mmol) was added hydrogen bromide in acetic acid (3 mL of a 33% by weight solution). The resulting mixture was stirred at reflux for 4 hours. The mixture was then partitioned between diethyl ether (25 mL) and saturated sodium hydrogen carbonate solution (25 mL). The organics were further washed with water (25 mL), brine (25 mL), dried over magnesium sulphate, filtered and concentrated under reduced pressure. The resulting precipitate was washed with pentane (10 mL) and then dried under reduced pressure to afford the title compound as a white solid in 88% yield, 82 mg.

WORKUP

后处理

  1. temperatureat reflux for 4 hours
  2. customThe mixture was then partitioned between diethyl ether (25 mL) and saturated sodium hydrogen carbonate solution (25 mL)
  3. washThe organics were further washed with water (25 mL), brine (25 mL)
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. washThe resulting precipitate was washed with pentane (10 mL)
  8. customdried under reduced pressure