反应详情

To a solution of 1.76 g of Pyrazol-1-yl-acetic acid in 20 ml of dry DMF 2.09 g of HOAT, 3.75 g of EDC and 6.9 ml of DIPEA were added at 0° C. After 30 min 3.3 g of 3-amino-4-(1-ethyl-propylamino)-benzoic acid methyl ester were added and the reaction was stirred at rt for 16 h. The reaction was then poured into water and extracted with ethyl acetate three times. The combined organic phases were washed with saturated aqueous sodium bicarbonate solution and brine, dried over magnesium sulphate and concentrated. The crude product was purified by precipitation from heptane to yield 2.28 g (47%) of 4-(1-Ethyl-propylamino)-3-(2-pyrazol-1-yl-acetylamino)-benzoic acid methyl ester.

1. extractionextracted with ethyl acetate three times
2. washThe combined organic phases were washed with saturated aqueous sodium bicarbonate solution and brine
3. dry with materialdried over magnesium sulphate
4. concentrationconcentrated
5. customThe crude product was purified by precipitation from heptane