HRID626742

反应详情

EQUATION

反应方程式

HRID 626742 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of [1-(4-azido-5-fluoropyridin-3-yl)-meth-(E)-ylidene]-(2,6-dichloro-4-fluorophenyl)-amine (14.7 mmol) in toluene (40 mL) was heated under reflux for 16 hours then allowed to cool to room temperature. The reaction mixture was concentrated under reduced pressure. The residue was purified by silica gel flash chromatography (0-50% ethyl acetate in cyclohexane) to afford the title compound as an off-white solid (3.38 g, 77% yield). LCMS (Method D): RT=2.84 min, m/z: 300 [M+H+].

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customThe residue was purified by silica gel flash chromatography (0-50% ethyl acetate in cyclohexane)