HRID1077360
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
A solution of 3.5 g. of 4-methylaminocyclohexanone, 5.1 g. of 2,4-difluorophenylhydrazine hydrochloride, and 4 g. of methanesulfonic acid in 50 ml. of absolute ethyl alcohol was heated under reflux for four hours, cooled, and filtered. The resulting solids were washed with isopropanol and treated in chloroform with 10% potassium hydroxide solution. The chloroform extract was evaporated to dryness to give 3-(methylamino)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole, m.p. 135°-138°C., which was converted to the hydrochloride salt, m.p. >280°C.
WORKUP
后处理
- temperatureunder reflux for four hours
- temperaturecooled
- filtrationfiltered
- washThe resulting solids were washed with isopropanol
- additiontreated in chloroform with 10% potassium hydroxide solution
- extractionThe chloroform extract
- customwas evaporated to dryness