反应详情

p-Bromobenzoic acid (6 g) and 3.35 g of triethylamine were dissolved in 80 ml of chloroform, the mixture was cooled at 0°-5° C. with stirring, and 3.26 g of ethyl chlorocarbonate was dropped thereinto. The mixture was stirred at the same temperature for 30 minutes, 5.86 g of methyl 4-(2-aminoethoxy)benzoate was added, and the mixture was stirred for 7 hours more. The reaction solution was washed with 10% hydrochloric acid, saturated potassium carbonate solution, and with water, dried with anhydrous magnesium sulphate, concentrated in vacuo, the residue was crystallised with n-hexane, and 8.5 g of crystals obtained were recrystallised from ethyl acetate to give 6.4 g of the product, m.p. 134°-136° C.

1. temperaturethe mixture was cooled at 0°-5° C.
2. stirringThe mixture was stirred at the same temperature for 30 minutes
3. stirringthe mixture was stirred for 7 hours more
4. washThe reaction solution was washed with 10% hydrochloric acid, saturated potassium carbonate solution
5. dry with materialwith water, dried with anhydrous magnesium sulphate
6. concentrationconcentrated in vacuo
7. customthe residue was crystallised with n-hexane, and 8.5 g of crystals
8. customobtained
9. customwere recrystallised from ethyl acetate