HRID447919

反应详情

EQUATION

反应方程式

HRID 447919 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Preparation took place analogously to Example 3 by reaction of 140 mg (0.52 mmol) N-[[(2,6-dimethoxybenzyl)amino](imino)methyl]thiourea with 140 mg (0.52 mmol) 4-(trifluoromethyl)phenacyl bromide. The educts were suspended in 3 ml dioxane, were added to 0.3 ml acetic acid and were heated for 40 minutes in the microwave (radiation 300 Watt). The mixture was subsequently concentrated and the crude product obtained was purified by chromatography on silica gel (dichloromethane/methanol 1-4%). Stirring of the yellow foam obtained with methyl tert.-butyl ether yielded 120 mg of a white amorphous solid.

WORKUP

后处理

  1. customPreparation
  2. temperaturewere heated for 40 minutes in the microwave (radiation 300 Watt)
  3. concentrationThe mixture was subsequently concentrated
  4. customthe crude product obtained
  5. customwas purified by chromatography on silica gel (dichloromethane/methanol 1-4%)
  6. customobtained with methyl tert.-butyl ether