HRID1666165

反应详情

EQUATION

反应方程式

HRID 1666165 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

16.3 g (74 mmol) of N-[2-(4-ethylphenyl)-1,1-dimethylethyl]acetamide and 8.0 g of potassium hydroxide are refluxed for 15 hours in 60 mL ethylene glycol. The reaction mixture is combined with ice water and extracted three times with diethyl ether. The combined organic phases are washed with water, dried with sodium sulfate, and freed from solvent. To prepare the hydrochloride, the crude product is dissolved in acetonitrile and ethereal hydrochloric acid and diethyl ether are added successively. The solid precipitated is suction filtered and dried. Yield: 11.0 g (69%, hydrochloride); melting point 165° C.-167° C.

WORKUP

后处理

  1. extractionextracted three times with diethyl ether
  2. washThe combined organic phases are washed with water
  3. dry with materialdried with sodium sulfate
  4. customTo prepare the hydrochloride
  5. customThe solid precipitated
  6. filtrationfiltered
  7. customdried