HRID1667658

反应详情

EQUATION

反应方程式

HRID 1667658 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 7.35 g (26.58 mmole) of 2-bromo-3-(4-chloro-phenyl)-3-oxo-propionamide and 300 mL of ethanol was added 2.02 g (26.58 mmole) of thiourea. The mixture was stirred at room temperature for 4 hours and then concentrated under reduced pressure. The residue was purified by silica gel chromatography, eluting with ethyl acetate-dichloromethane (1:3, then 3:1, then 1:0). Recrystallization of the residue gave 1.11 g of 2-amino-4-(4-chloro-phenyl)-thiazole-5-carboxylic acid amide (V.18) as pale yellow crystals.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. customThe residue was purified by silica gel chromatography
  3. washeluting with ethyl acetate-dichloromethane (1:3
  4. customRecrystallization of the residue