反应详情

To a solution of 4.3 g (0.03 mole) 1-carbomethoxypiperazine in 10 ml of ethanol was added 10.0 g (0.036 mole) of 4-chloro-1,1-bis-(p-fluorophenyl)-butane and 5.0 g of sodium bicarbonate. The mixture was heated at reflux for 36 hours. 100 ml of water was added. The mixture was extracted twice with Et2O. The combined extracts were dried over sodium sulphate and concentrated. The residue was dissolved in ethanol-ether and the hydrochloride was precipitated with ethanolic HCl. The solid was collected by filtration and recrystallised from propan-2-ol to give 2.2 g of 1-carbomethoxy-4-[4,4-bis(p-fluorophenyl)butyl]-piperazine hydrochloride. Melting point 192°-193° C.

1. temperatureThe mixture was heated
2. temperatureat reflux for 36 hours
3. extractionThe mixture was extracted twice with Et2O
4. dry with materialThe combined extracts were dried over sodium sulphate
5. concentrationconcentrated
6. dissolutionThe residue was dissolved in ethanol-ether
7. customthe hydrochloride was precipitated with ethanolic HCl
8. filtrationThe solid was collected by filtration
9. customrecrystallised from propan-2-ol