HRID614495
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
Phenoxathiin (22.9 g) and acetyl chloride (8.8 ml) were dissolved in carbon disulphide (120 ml) and mechanically stirred while aluminum chloride (15.5 g) was added in small portions. The red mixture was stirred for 2 hr. at room temperature, then boiled under reflux on the water bath for a further 21/4 hr. The mixture was cooled and poured on to ice and hydrochloric acid, and the precipitated product filtered off, washed with water, and recrystallised once from ethanol and twice from petroleum ether (b.p. 80°-100° C) to give the product m.p. 112° C.
WORKUP
后处理
- additionwas added in small portions
- customat room temperature
- temperatureThe mixture was cooled
- filtrationthe precipitated product filtered off
- washwashed with water
- customrecrystallised once from ethanol and twice from petroleum ether (b.p. 80°-100° C)