反应详情

温度

100 °C

To a solution of 1.5 g of 4-{(S)-4-tert-Butoxycarbonyl-2-[(5-hydroxy-1-phenyl-1H-pyrazole-3-carbonyl)-amino]-butyryl}-piperazine-1-carboxylic acid ethyl ester in 20 ml of DMF, 1.8 g of cesium carbonate and 1.2 g of 1-Bromo-cyclobutanecarboxylic acid ethyl ester was added and heated to 100° C. for 2 h. Then, the reaction mixture was diluted with water and extracted with ethyl acetate (3×150 ml). The combined organic phases were dried over MgSO4 and the solvents were removed under reduced pressure. The crude product was purified by chromatography on silica gel eluting with a gradient of n-heptane/ethyl acetate. The fractions containing the product were combined and the solvent evaporated under reduced pressure. Yield: 860 mg.

1. extractionextracted with ethyl acetate (3×150 ml)
2. dry with materialThe combined organic phases were dried over MgSO4
3. customthe solvents were removed under reduced pressure
4. customThe crude product was purified by chromatography on silica gel eluting with a gradient of n-heptane/ethyl acetate
5. additionThe fractions containing the product
6. customthe solvent evaporated under reduced pressure