反应详情

To a mixture of 4-(9-cyclopentyl-7,7-difluoro-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino)-3-methoxy-N-(1-methylpiperidin-4-yl)benzamide (543 mg, 1 mmol) in 10 ml of DMF, was added 1N NaOH (5 ml) dropwise. The reaction mixture was stirred at rt. for 1 h and then subjected to reverse phase HPLC purification using basic column. The final compound was obtained by lyophilization first and then dried in the vacuum oven at 60° C. for 3 d (380 mg, 68%). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.47-1.99 (m, 12 H) 2.54 (d, J=2.8 Hz, 2 H) 2.64-2.79 (m, 5 H) 3.00 (d, J=4.6 Hz, 2 H) 3.85-4.10 (m, 6 H) 4.20 (d, J=7.3 Hz, 1 H) 7.42 (s, 2 H) 7.48 (d, J=8.3 Hz, 1 H) 7.61-7.80 (m, 1 H) 8.23 (br. s., 1 H) 8.42 (d, J=8.3 Hz, 1 H). [M+H] calc'd for C27H37F2N7O4, 562; found 562.

1. customphase HPLC purification