反应 #215303

反应方程式

4-methylaminocyclohexanone

2,4-difluorophenylhydrazine hydrochloride

methanesulfonic acid

→

3-(methylamino)-6,8-difluoro-1,2,3,4-tetrahydrocarbazole

溶剂

ethyl alcohol

反应条件

后处理

1. 1
   温度under reflux for four hours
2. 2
   温度cooled
3. 3
   过滤filtered
4. 4
   洗涤The resulting solids were washed with isopropanol
5. 5
   workup.ADDITIONtreated in chloroform with 10% potassium hydroxide solution
6. 6
   萃取The chloroform extract
7. 7
   其他was evaporated to dryness

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.

来源