HRID1827410
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe reaction mixture is refluxed for 2 h
- temperaturereflux
- temperatureThe mixture is cooled
- waithold overnight in the frig
- filtrationThe precipitate is filtered off
- customrecrystallised from methanol
- customto yield 0.043 g (12%) of filthy, colorless needles