反应详情

温度

40 °C

To a solution of 4.2 g (5.19 mmol) of 1,3-bis[4-[4-(3,5-dimethoxy-4-propoxyphenyl) benzoyl]-1-piperazinyl]propane in methanol (30 mL) stirred in an ice bath, was added 3.2 mL (13 mmol) of a 4.0 mol/L ethyl acetate solution of hydrogen chloride, and the mixture was concentrated under reduced pressure. Methanol (50 mL) was added and the mixture was concentrated under reduced pressure again. A suspension of the residue in methanol-chloroform (10:1, 44 mL) was stirred at 40° C. to give a homogeneous solution. Diethyl ether (10 mL) was added to the solution and the mixture was stirred at room temperature and at 0° C. Precipitates were collected by filtration and washed successively with methanol-diethyl ether (2:3) and diethyl ether to afford 3.92 g of 1,3-bis[4-[4-(3,5-dimethoxy-4-propoxyphenyl) benzoyl)-1-piperazinyl]propane dihydrochloride as a colorless crystalline powder (yield: 86%).

1. concentrationthe mixture was concentrated under reduced pressure
2. additionMethanol (50 mL) was added
3. concentrationthe mixture was concentrated under reduced pressure again
4. additionA suspension of the residue in methanol-chloroform (10:1, 44 mL)
5. customto give a homogeneous solution
6. stirringthe mixture was stirred at room temperature and at 0° C
7. customPrecipitates
8. filtrationwere collected by filtration
9. washwashed successively with methanol-diethyl ether (2:3) and diethyl ether