HRID1767749
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe reaction heated
- temperatureat reflux for 2 hours
- custombefore quenching by the addition of methanol (1 ml)
- customPurification by flash chromatography on silica gel
- washeluting with 12% ethyl acetate in isohexane