反应详情

To a suspension of tert-butyl {3-[4-(2-phenyl-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl)phenyl]oxetan-3-yl}carbamate (29 mg) in dichloromethane (4 mL) was added trifluoroacetic acid (2 mL) at 0° C. dropwise. After being stirred at room temperature for 1 h, the reaction mixture was concentrated under reduced pressure. Purification by column chromatography (NH-silica gel: 0-3% methanol in chloroform) gave the product (16 mg, 68%). 1HNMR (DMSO-d6) 400 MHz δ: 8.57 (s, 1H), 8.08 (dd, J=4.8, 1.6 Hz, 1H), 7.96 (dd, J=7.8, 1.4 Hz, 1H), 7.61 (d, J=8.3 Hz, 2H), 7.53-7.49 (m, 2H), 7.38-7.21 (m, 7H), 7.12 (t, J=7.6 Hz, 1H), 6.90 (dd, J=8.0, 1.6 Hz), 6.74 (dd, J=8.0, 4.8 Hz, 1H), 4.71-4.65 (m, 4H). LCMS: 458 [M+H].

1. concentrationthe reaction mixture was concentrated under reduced pressure
2. customPurification by column chromatography (NH-silica gel: 0-3% methanol in chloroform)