反应详情

温度

60 °C

Sodium hydride (3.59 g of 60% in oil) is added to 4-hydroxybenzaldehyde (9.95 g) in dimethylformamide (250 mL) and the mixture stirred at 60° C. for 30 minutes. 1-(3-Chloropropyl)-4-phenylpiperazine (Step A) (19.5 g) is added and the mixture stirred for 14 hours at 60° C. The solvent is evaporated and the residue treated with water (300 mL) and extracted with dichloromethane (3×150 mL). The extracts are dried over magnesium sulfate, filtered and evaporated to leave a beige solid. This solid is recrystallized from ethyl acetate/diethyl ether to give 18.4 g of the title compound as a light beige solid.

1. stirringthe mixture stirred for 14 hours at 60° C
2. customThe solvent is evaporated
3. additionthe residue treated with water (300 mL)
4. extractionextracted with dichloromethane (3×150 mL)
5. dry with materialThe extracts are dried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. customto leave a beige solid
9. customThis solid is recrystallized from ethyl acetate/diethyl ether