HRID1375020

反应详情

EQUATION

反应方程式

HRID 1375020 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1-acetyl-3-[[3-methoxy-4-(trifluoromethyl)phenyl]methylene]piperazine-2,5-dione (1.8 g) in tetrahydrofuran (50 ml) was hydrogenated over 10% palladium-carbon (50% wet, 180 mg) for 5 hours at atmospheric pressure. After removal of the catalyst by filtration, the filtrate was added hydrazine monohydrate (395 mg). The mixture was stirred for 1.5 hours at room temperature and concentrated under reduced pressure. The residue was triturated with isopropyl ether (12 ml) and the precipitates were collected by filtration, and washed with isopropyl ether to give 3-[3-methoxy-4-(trifluoromethyl)benzyl]piperazine-2,5-dione (1.29 g) as a powder.

WORKUP

后处理

  1. customAfter removal of the catalyst
  2. filtrationby filtration
  3. additionthe filtrate was added hydrazine monohydrate (395 mg)
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was triturated with isopropyl ether (12 ml)
  6. filtrationthe precipitates were collected by filtration
  7. washwashed with isopropyl ether