HRID908193

反应详情

EQUATION

反应方程式

HRID 908193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

1-(4-Methanesulfonyl-3-trifluoromethyl-phenyl)-propan-2-one (Example 59c) (0.60 g, 2.14 mmol) is dissolved in dioxan (50 ml) and the solution is cooled to 10° C. at which point the mixture is semi frozen. Bromine (0.088 ml, 1.7 mmol) is added slowly and the mixture is stirred for an additional 30 min in a semi frozen state. The mixture is then allowed to warm to room temperature and the solvent is removed to give a brown oil. This material is dissolved in ethanol and pyrazin-2-yl-thiourea (1a) is added in one portion. The mixture is stirred at 60° C. for 30 minutes then allowed to cool whereupon the titled product precipitates and is removed by filtration.

WORKUP

后处理

  1. temperatureis semi frozen
  2. temperaturefrozen state
  3. temperatureto warm to room temperature
  4. customthe solvent is removed
  5. customto give a brown oil
  6. stirringThe mixture is stirred at 60° C. for 30 minutes