HRID476560
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureat reflux for 3 days
- temperatureAfter cooling
- customthe insoluble inorganic material removed by filtration
- concentrationthe filtrate concentrated under reduced pressure
- customThe resulting oil was purified by flash chromatography on silica gel eluting with ether (93)