HRID4809

反应详情

EQUATION

反应方程式

HRID 4809 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9.55 g of phosphorus pentasulfide and 9.5 g of potassium sulfide were ground together and added to a solution of 20.2 g (0.07 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,1-f][1,4]oxazepin-5(4H)-one in 200 ml of dry toluene. The mixture was stirred and heated at reflux for 7 hr. The hot reaction mixture was filtered and the product crystallized from the cooled filtrate. Recrystallization from chloroform gave 18 g (84%) of yellow crystals, m.p. 167°-170° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 7 hr
  3. filtrationThe hot reaction mixture was filtered
  4. customthe product crystallized from the cooled filtrate
  5. customRecrystallization from chloroform