反应详情

The ketone prepared as described above (5.4 g) was mixed with N-methylformamide (18 ml), 98% formic acid (4 ml) and 25% aqueous methylamine (0.6 ml) and the mixture heated under reflux for sixteen hours. The mixture was poured into water and extracted with dichloromethane. The extract was washed, dried and evaporated to give a residue which was heated under reflux with concentrated hydrochloric acid (10 ml) for six hours. The mixture was evaporated to dryness and the residue dried by repeated addition and vacuum evaporation of an industrial methylated spirit/toluene mixture. The solid residue was recrystallised from propan-2-ol to give N-methyl-2-[1-(4-chlorophenyl)-cyclobutyl]-1-methylethylamine hydrochloride (m.p. 193°-194° C.) (Formula I R1, R2 =H; R3 =Me; R4 =H; R5 =4-Cl; R6 =H; R7 =Me; R8 =H).

1. temperaturethe mixture heated
2. temperatureunder reflux for sixteen hours
3. extractionextracted with dichloromethane
4. washThe extract was washed
5. customdried
6. customevaporated
7. customto give a residue which
8. temperaturewas heated
9. customThe mixture was evaporated to dryness
10. customthe residue dried
11. additionaddition and vacuum evaporation of an industrial methylated spirit/toluene mixture
12. customThe solid residue was recrystallised from propan-2-ol