HRID476560

反应详情

EQUATION

反应方程式

HRID 476560 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of benzothiazol-2-yl-piperazine (0.4 g, 1.55 mmole), 2-(2,4-dichlorophenyl)-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane methanesulphonate (see EP-A-44605) (0.57 g, 1.55 mmole) and potassium carbonate (2 g, 14 mmole) in dioxan (20 ml) was heated at reflux for 3 days. After cooling, the mixture was diluted with methylene chloride, the insoluble inorganic material removed by filtration and the filtrate concentrated under reduced pressure. The resulting oil was purified by flash chromatography on silica gel eluting with ether (93): ethanol (7): 0.88 ammonia solution (1) to yield the desired product as a foam, m.p. 68°-85° (0.34 g, 44%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 3 days
  3. temperatureAfter cooling
  4. customthe insoluble inorganic material removed by filtration
  5. concentrationthe filtrate concentrated under reduced pressure
  6. customThe resulting oil was purified by flash chromatography on silica gel eluting with ether (93)