反应详情

To a suspension of tert-butyl {1-[4-(2-phenyl-9H-imidazo[1,2-d]pyrido[2,3-b][1,4]benzodiazepin-3-yl)phenyl]cyclopropyl}carbamate (27 mg) in dichloromethane (4 mL) was added trifluoroacetic acid (2 mL) at 0° C. dropwise. After being stirred at room temperature for 30 min, the reaction mixture was concentrated under reduced pressure. Purification by column chromatography (NH-silica gel: 10-100% chloroform in hexanes then 10% methanol in chloroform) gave the product (25 mg, quant.). 1HNMR (DMSO-d6) 400 MHz δ: 8.54 (s, 1H), 8.07 (dd, J=4.8, 1.6 Hz, 1H), 7.95 (dd, J=7.8, 1.4 Hz, 1H), 7.49 (d, J=6.9 Hz, 2H), 7.38-7.20 (m, 7H), 7.14-7.07 (m, 3H), 6.90 (dd, J=8.0, 1.6 Hz, 1H), 6.75 (dd, J=8.0, 4.8 Hz, 1H), 1.06-1.00 (m, 2H), 0.99-0.93 (m, 2H). LCMS: 442 [M+H].

1. concentrationthe reaction mixture was concentrated under reduced pressure
2. customPurification by column chromatography (NH-silica gel
3. custom10-100% chloroform in hexanes then 10% methanol in chloroform) gave the product (25 mg, quant.)