反应详情

An opaque solution of 2-({2-chloro-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-4,6-difluorobenzoic acid (5.3 g, 11.07 mmol) in THF (300 mL) was treated with a few drops of DMF, followed by oxalyl chloride (1M in CH2Cl2, 22.14 mL, 44.3 mmol). The reaction mixture was stirred for 1 h, then placed in an ice-bath for 2 h. The resulting slurry was filtered, the solid washed with CH2Cl2 to obtain 5-chloro-8,10-difluoro-3-[(4-methylphenyl)sulfonyl]pyrrolo[2′,3′:4,5]pyrimido[6,1-b]quinazolin-7(3H)-one hydrogen chloride as a white solid (5.23 g, 95%). 1H NMR (400 MHz, THF-d6) δ ppm 2.41 (s, 3H), 6.97-7.12 (m, 2H), 7.12-7.24 (m, 1H), 7.44 (d, J=8.24 Hz, 2H), 7.68 (d, J=3.66 Hz, 1H), 8.11 (d, J=8.42 Hz, 2H); ESIMS (M+H)+=460.94.

1. waitplaced in an ice-bath for 2 h
2. filtrationThe resulting slurry was filtered
3. washthe solid washed with CH2Cl2