反应详情

To a solution of triphosgene (0.30 g, 1 mmol) in CH2Cl2 (70 ml) at −5° C. were added 3-bromo-4-fluoroaniline (0.19 g, 1 mmol) in CH2Cl2 (20 ml) and triethylamine (0.60 ml, 4.3 mmol). The reaction was stirred at room temperature for 20 min, then (S)-5-methyl-4-(3-methylpiperazin-1-yl)-7H-pyrrolo[2,3-d]pyrimidine from step B (0.23 g, 1 mmol) in CH2Cl2 (30 ml) was added. The mixture was stirred for 1.5 hours, then concentrated under vacuum. The residue was purified by prep HPLC to afford (S)—N-(3-bromo-4-fluorophenyl)-2-methyl-4-(5-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)piperazine-1-carboxamide (65 mg) as a white solid.

1. stirringThe mixture was stirred for 1.5 hours
2. concentrationconcentrated under vacuum
3. customThe residue was purified by prep HPLC