反应详情

To a solution of tert-butyl 4-(5-(3,5-dimethylisoxazol-4-yl)-2-oxo-3-phenylindolin-3-yl)piperazine-1-carboxylate (0.9 g, 1.8 mmol) in CH2Cl2 (5 mL) was added TFA (5 mL) at 0° C., after adding up, the reaction was stirred at room temperature for 2.0 h. The solvent was evaporated in vacuo to give crude product. It was dissolved in water (20 mL), and was neutralized with NaHCO3 to PH=7˜8, and then the mixture was extracted with EtOAc (2×30 mL), combined organic phase, dried with Na2SO4, filtrated, concentrated to give crude product, and the mixture was purified by chromatography (eluent. CH2Cl2/MeOH/NH3H2O=20/1/0.05) to give product (500 mg, 71.6%) as a white solid. 1H NMR (400 MHz, DMSO-d6): δH 10.75 (s, 1H), 7.49 (d, J=8.0 Hz, 2H), 7.23-7.36 (m, 5H), 6.97 (d, J=8.0 Hz, 1H), 2.65-2.66 (m, 4H), 2.31-2.47 (m, 7H), 2.19 (s, 3H). MS (ESI) m/e [M+1]+ 389.

1. additionafter adding up
2. customThe solvent was evaporated in vacuo
3. customto give crude product
4. extractionthe mixture was extracted with EtOAc (2×30 mL)
5. dry with materialdried with Na2SO4
6. filtrationfiltrated
7. concentrationconcentrated
8. customto give crude product
9. customthe mixture was purified by chromatography (eluent. CH2Cl2/MeOH/NH3H2O=20/1/0.05)