HRID2072020
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe solution was evaporated
- customto leave a colourless oil which
- temperaturecooling
- customprecipitated the hydrochloride as colourless prisms which
- dry with materialwas dried over potassium hydroxide in vacuo (0.688 g., m.p. 160°-170°)
- customRecrystallisation from ethanol (addition of ether)