反应详情

温度

85 °C

A mixture of 2,4-dichloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidine (25 g, 73.1 mmol), 2-aminobenzoic acid (10.02 g, 73.1 mmol) and DIPEA (63.8 mL, 365 mmol) in iPrOH (300 mL) was heated at 85° C. bath for 17 h. The resulting mixture was allowed to cool to rt and was concentrated to about half volume. EtOAc (400 mL) was added, followed by a 1N aqueous HCl solution (400 mL). The resulting slurry was filtered, the solids were washed with EtOAc and triturated using Et2O to obtain 2-({2-chloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)benzoic acid as a yellow solid (28.44 g 88%). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.36 (s, 3H), 7.11-7.23 (m, 1H), 7.47 (d. J=8.61 Hz, 2H), 7.56-7.67 (m, 1H), 7.76 (d, J=3.85 Hz, 1H), 7.95 (dd, J=7.69 Hz, 1.46 Hz, 1H), 7.97-8.02 (m, 2H), 8.29-8.36 (m, 1H), 11.36 (s, 1H); ESIMS (M+H)+=443.06.

1. temperatureto cool to rt
2. concentrationwas concentrated to about half volume
3. additionEtOAc (400 mL) was added
4. filtrationThe resulting slurry was filtered
5. washthe solids were washed with EtOAc
6. customtriturated