HRID1198633

反应详情

EQUATION

反应方程式

HRID 1198633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 190 ml of acetone and 36.0 g of sodium hydroxide in 600 ml of water was treated with 60.0 g of cyclopentanone under stirring. After stirring for about 12 hours at about room temperature, the mixture was neutralized with 36% acetic acid and extracted with three 60 ml portions of ether. The combined extracts were dried over anhydrous magnesium sulfate and evaporated to give a residue. The residue was distilled to obtain 62.6 g of 2-(1-methylethylidene) cyclopentanone as a colorless liquid. The boiling point of this intermediate compound was determined to be 85°-88° C. at a pressure of 10 mm Hg. A subsequent Mannich reaction yielded the 2-Dimethylaminomethyl-5-(1-methylethylidene) cyclopentanone hydrochloride. The melting point of the product was determined to be 173°-175° C.

WORKUP

后处理

  1. stirringAfter stirring for about 12 hours at about room temperature
  2. extractionextracted with three 60 ml portions of ether
  3. dry with materialThe combined extracts were dried over anhydrous magnesium sulfate
  4. customevaporated
  5. customto give a residue
  6. distillationThe residue was distilled