HRID1283564

反应详情

EQUATION

反应方程式

HRID 1283564 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Dimethylamino-N-[3,4-dichlorotolyl]-cyclohexane carboxamide (0.658 g.,) was dissolved in ethanol (5 ml.) and ethereal hydrogen chloride (10 ml.) was added. The solution was evaporated to leave a colourless oil which was taken up in the minimum volume of acetic acid. Dropwise addition of ether, with scratching and cooling, precipitated the hydrochloride as colourless prisms which was dried over potassium hydroxide in vacuo (0.688 g., m.p. 160-170°). Recrystallisation from ethanol (addition of ether) afforded 1-dimethylamino-N-[3,4-dichlorotolyl]-cyclohexane carboxamide hydrochloride as white prisms (0.351 g., 48%); m.p. 162-166°C.

WORKUP

后处理

  1. customThe solution was evaporated
  2. customto leave a colourless oil which
  3. temperaturecooling
  4. customprecipitated the hydrochloride as colourless prisms which
  5. dry with materialwas dried over potassium hydroxide in vacuo (0.688 g., m.p. 160-170°)
  6. customRecrystallisation from ethanol (addition of ether)