反应详情

Methyl 4-(2-aminoethoxy)benzoate (19.5 g) and 13.8 g of anhydrous potassium carbonate were added to 200 ml of chloroform and the mixture was stirred with cooling. p-Chlorobenzoyl chloride (17.5 g) was dropped thereinto at 10°-20° C. The mixture was stirred for 3 hours. The reaction solution was washed with water, the chloroform layer was dried with anhydrous magnesium sulphate, concentrated in vacuo, the residue was crystallised with n-hexane, and the crystals were recrystallised with ethyl acetate/n-hexane to give 25.4 g of crystals of m.p. 125°-127° C., yield 76%.

1. temperaturewith cooling
2. customat 10°-20° C
3. stirringThe mixture was stirred for 3 hours
4. washThe reaction solution was washed with water
5. dry with materialthe chloroform layer was dried with anhydrous magnesium sulphate
6. concentrationconcentrated in vacuo
7. customthe residue was crystallised with n-hexane
8. customthe crystals were recrystallised with ethyl acetate/n-hexane