HRID1767749

反应详情

EQUATION

反应方程式

HRID 1767749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium hydride (60% dispersion in oil-50 mg, 1.25 mmol) was added to a solution of 3-chloro-4-fluorobenzyl alcohol (177 mg, 1.1 mmol) in tetrahydrofuran (5 ml) under an atmosphere of nitrogen. After 10 minutes, 2-chloro-5-nitropyrimidine (159 mg, 1 mmol) was added and the reaction heated at reflux for 2 hours before quenching by the addition of methanol (1 ml). Purification by flash chromatography on silica gel, eluting with 12% ethyl acetate in isohexane yielded the title compound (86 mg, 30% yield):

WORKUP

后处理

  1. temperaturethe reaction heated
  2. temperatureat reflux for 2 hours
  3. custombefore quenching by the addition of methanol (1 ml)
  4. customPurification by flash chromatography on silica gel
  5. washeluting with 12% ethyl acetate in isohexane