反应详情

p-tert-Butylbenzoic acid (5.35 g) and 3.34 g of triethylamine were dissolved in 70 ml of chloroform and 3.26 g of ethyl chloroformate was dropped into the above mixture with stirring and cooling at 0° to 5° C. After the dropping, the mixture was stirred at the same temperature for 30 minutes and, after addition of 5.86 g of methyl 4-(2-aminoethoxy)benzoate thereto, the mixture was stirred for 6 hours more. The reaction solution was washed with 10% hydrochloric acid, saturated potassium carbonate solution, and water, dried with anhydrous magnesium sulpahte, concentrated in vacuo, and the residue was crystallised with n-hexane to give 9.8 g of crystals which were further recrystallised from ethyl acetate to give 7.64 g (yield: 71.65%) of the product, m.p. 112°-114° C.

1. temperaturecooling at 0° to 5° C
2. stirringAfter the dropping, the mixture was stirred at the same temperature for 30 minutes
3. stirringthe mixture was stirred for 6 hours more
4. washThe reaction solution was washed with 10% hydrochloric acid, saturated potassium carbonate solution, and water
5. dry with materialdried with anhydrous magnesium sulpahte
6. concentrationconcentrated in vacuo
7. customthe residue was crystallised with n-hexane