HRID1507466

反应详情

EQUATION

反应方程式

HRID 1507466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 3-(2-Fluoro-4-methoxyphenyl)-3-oxopropanenitrile (9.55 g, 49.4 mmol) suspended in ethanol (165 mL) was added hydrazine hydrate (1.743 g, 54.38 mmol). The resulting mixture was heated at reflux overnight. Then, the organic solvent was evaporated in vacuo and the resulting residue was chromatographed (eluting with 9:1 methylene chloride:methanol) to give 9.07 g (88% yield) of the title compound. LCMS (ESI): calc.=207; obs. M+H=208.2.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux overnight
  3. customThen, the organic solvent was evaporated in vacuo
  4. customthe resulting residue was chromatographed
  5. wash(eluting with 9:1 methylene chloride:methanol)