反应详情

温度

180 °C

A mixture of 1-[1-(4-chlorophenyl)cyclobutyl]propan-2-one prepared as described in Example 3 (15 g) and 98% formic acid (4 ml) was added dropwise to formamide (12 ml) at 160° C. The temperature was raised to 180° C. and maintained at this temperature for ten hours. The mixture was cooled, diluted with water and extracted with dichloromethane. The extract was washed, dried and evaporated to yield a yellow oil which was hydrolysed with concentrated hydrochloric acid under reflux. The resulting aqueous solution after dilution with water was washed with ether, aqueous NaOH was added and the aqueous solution extracted with ether. The extracts were washed, dried and evaporated to yield a residue which on distillation gave 2-[1-(4-chlorophenyl)cyclobutyl]-1-methylethylamine (b.p. 105°-107°/0.7 mm Hg).

1. customprepared
2. temperaturemaintained at this temperature for ten hours
3. temperatureThe mixture was cooled
4. extractionextracted with dichloromethane
5. washThe extract was washed
6. customdried
7. customevaporated
8. customto yield a yellow oil which
9. temperatureunder reflux
10. washThe resulting aqueous solution after dilution with water was washed with ether, aqueous NaOH
11. additionwas added
12. extractionthe aqueous solution extracted with ether
13. washThe extracts were washed
14. customdried
15. customevaporated
16. customto yield a residue which
17. distillationon distillation