HRID614495

反应详情

EQUATION

反应方程式

HRID 614495 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. additionwas added in small portions
  2. customat room temperature
  3. temperatureThe mixture was cooled
  4. filtrationthe precipitated product filtered off
  5. washwashed with water
  6. customrecrystallised once from ethanol and twice from petroleum ether (b.p. 80°-100° C)