HRID1475941

反应详情

EQUATION

反应方程式

HRID 1475941 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 3-(4-methoxyphenyl)-3-oxopropanenitrile (5.0 g, 28.5 mmol) in ethanol (100 mL) was added hydrazine hydrate (2.8 mL, 57.1 mmol) at room temperature. The mixture was heated to reflux for 8 h, allowed to cool and concentrated under reduced pressure to about ¼ volume (25 mL). The resulting precipitate was allowed to stir overnight at room temperature, filtered and rinsed with ethanol (2 mL). The title product was dried under vacuum. Yield 4.15 g (77%); LCMS m/z 190.1 (M+H)+, ret. time=1.56 min.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 8 h
  3. temperatureto cool
  4. concentrationconcentrated under reduced pressure to about ¼ volume (25 mL)
  5. filtrationfiltered
  6. washrinsed with ethanol (2 mL)
  7. dry with materialThe title product was dried under vacuum