反应详情

To a solution of 2-({2-chloro-6-methyl-7-[(4-methylphenyl)sulfonyl]-7H-pyrrolo[2,3-d]pyrimidin-4-yl}amino)-6-fluorobenzoic acid (439 mg, 0.924 mmol) in THF (15 mL) and DMF (few drops) was added 2M oxalyl chloride solution in dichloromethane (0.56 mL, 1.13 mmol) dropwise. After ˜15 min, LCMS analysis shows reaction complete so reaction mixture was cooled in an ice bath and filtered via a buchner funnell and thet solid was washed with THF and dried under reduced pressure to afford 5-chloro-8-fluoro-2-methyl-3-[(4-methylphenyl)sulfonyl]pyrrolo[2′,3′:4,5]pyrimido[6,1-b]quinazolin-7(3H)-one HCl salt (423 mg, 0.86 mmol) as a yellow solid. ESIMS (M+H)+=457.

1. customreaction
2. customcomplete so reaction mixture
3. temperaturewas cooled in an ice bath
4. filtrationfiltered via a buchner funnell
5. washthet solid was washed with THF
6. customdried under reduced pressure