HRID1827410

反应详情

EQUATION

反应方程式

HRID 1827410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 0.35 g (1.1 mmol) of N-[4-(3-fluoro-benzyloxy)-phenyl]-malonamic acid methyl ester in 7 ml methanol is treated with 83 mg (1.7 mmol) of hydrazine hydrate. The reaction mixture is refluxed for 2 h, then another portion of 300 mg (6 mmol) of hydrazine hydrate is added and reflux is pursued for another 8 h. The mixture is cooled and hold overnight in the frig. The precipitate is filtered off and recrystallised from methanol to yield 0.043 g (12%) of filthy, colorless needles. MS: m/e=318.3 (M++H).

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 2 h
  2. temperaturereflux
  3. temperatureThe mixture is cooled
  4. waithold overnight in the frig
  5. filtrationThe precipitate is filtered off
  6. customrecrystallised from methanol
  7. customto yield 0.043 g (12%) of filthy, colorless needles