HRID1993404

反应详情

EQUATION

反应方程式

HRID 1993404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 4-(6-oxo-1,6-dihydro-pyrimidin-4-yl)-piperazine-1-carboxylic acid benzyl ester (Intermediate 3; 2.00 g, 7.14 mmol) and a catalytic amount of 10% palladium on carbon in ethanol (300 mL) was hydrogenated at atmospheric temperature and pressure. The starting material is not readily soluble in ethanol so it is clearly visible. After 6 h, the amount of starting material was significantly reduced. Hydrogenation was continued overnight, and a large amount of solid was present. Acetonitrile (300 mL) was added and the mixture was heated to dissolve the solid. The catalyst was filtered off using Celite, and the solvent was evaporated from the filtrate to give 6-piperazin-1-yl-3H-pyrimidin-4-one (820 mg, 64%) as a white solid.

WORKUP

后处理

  1. waitHydrogenation was continued overnight
  2. temperaturethe mixture was heated
  3. dissolutionto dissolve the solid
  4. filtrationThe catalyst was filtered off
  5. customthe solvent was evaporated from the filtrate