反应详情

温度

85 °C

Phenyl N′-cyano-N-(3-fluorophenyl)carbamimidate, prepared analogously to phenyl N-3-chlorophenyl-N′-cyanocarbamimidate from Example 6, step A, (0.55 g, 2.2 mmol), (S)-5-methyl-4-(3-methylpiperazin-1-yl)-7H-pyrrolo[2,3-d]pyrimidine, from example 1, step B, (0.50 g, 2.2 mmol), and N,N-diisopropylethylamine (1 ml) were added to acetonitrile (10 ml). The mixture was heated at 85° C. in a sealed pressure tube for 4 hours. The solvent was evaporated, and the residue was purified prep HPLC (Sunfire C18 30×250 mm column. 10-100% MeCN:H2O (10 mM NH4OAc), 18 min., 45 ml/min) to give (S)—N′-cyano-N-(3-fluorophenyl)-2-methyl-4-(5-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)piperazine-1-carboximidamide (0.23 g, 0.58 mmol, 27%).

1. customThe solvent was evaporated
2. customthe residue was purified prep HPLC (Sunfire C18 30×250 mm column. 10-100% MeCN:H2O (10 mM NH4OAc), 18 min., 45 ml/min)