HRID614698

反应详情

EQUATION

反应方程式

HRID 614698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

30.5 g (0.27 mol) of chlorobenzene and 36 g (0.27 mol) of aluminium chloride are introduced into a 250 cm3 flask and 25 g (0.135 mol) of m-nitrobenzoyl chloride dissolved in 15 cm3 of chlorobenzene are added dropwise. The mixture is heated for 5 hours at between 50° and 60° C. and is then allowed to cool and is hydrolysed with 500 g of ice + 20 cm3 of concentrated HCl (d = 1.18); the batch is extracted with ether and the extract is washed with aqueous sodium hydroxide solution (strength 30 g/l) and then with water; the ether phase is dried, decolorised and then evaporated in vacuo; 26 g of the expected ketone are obtained. Melting point 97° C.

WORKUP

后处理

  1. additionare added dropwise
  2. temperatureThe mixture is heated for 5 hours at between 50° and 60° C.
  3. temperatureto cool
  4. extractionthe batch is extracted with ether
  5. washthe extract is washed with aqueous sodium hydroxide solution (strength 30 g/l)
  6. dry with materialthe ether phase is dried
  7. customevaporated in vacuo