HRID904667

反应详情

EQUATION

反应方程式

HRID 904667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The product of step (b) (3 g, 0.0099 mole) was dissolved in dry benzene (50 mls), treated with phosphoryl chloride (2.5 mls) and refluxed for 1 hour. The reaction mixture was cooled, poured into water and extracted with ether, which was then washed with water and dried over magnesium sulphate. The solvent was evaporated to leave 2.8 g of yellow-brown solid. Recrystallisation from cyclohexane gave yellow needles mp 163°-164°.

WORKUP

后处理

  1. temperaturerefluxed for 1 hour
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with ether, which
  4. washwas then washed with water
  5. dry with materialdried over magnesium sulphate
  6. customThe solvent was evaporated