HRID75522

反应详情

EQUATION

反应方程式

HRID 75522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-fluoro-4-formylbenzonitrile 1 (100 mg, 0.7 mmol) and 4,5-dimethyl benzene-1,2-diamine 2 (109 mg, 0.8 mmol) in ethanol (10 ml) was added a catalytic amount of p-toluenesulfonic acid (0.5 mg, 0.5 mmol). The mixture was stirred reflux for 2 hours and concentrated by rotor evaporation. The crude material was purified through column chromatography with 40% ethyl acetate in hexane to yield compound 3 as white solid (68% yield, 121 mg, confirmed by LCMS: 266.20).

WORKUP

后处理

  1. temperaturereflux for 2 hours
  2. concentrationconcentrated by rotor evaporation
  3. customThe crude material was purified through column chromatography with 40% ethyl acetate in hexane