反应详情

温度

105 °C

A mixture of N-(2,2-dimethoxyethyl)-11H-pyrido[2,3-b][1,4]benzodiazepin-6-amine (4.21 g, 14 mmol) and acetic acid (20 mL) was heated to 105° C. for 13 hours. After cooling to room temperature the solvent was removed under reduced pressure. The resulting crude product was diluted with acetone and filtered by suction to give a dark pink solid (74%). 1H NMR (DMSO-d6) 400 MHz δ: 8.53 (s, 1H), 8.15 (dd, J=4.6, 1.7 Hz, 1H), 7.85 (dd, J=7.7, 1.4 Hz, 1H), 7.77 (dd, J=7.7, 1.4 Hz, 1H), 7.63 (d, J=1.2 Hz, 1H), 7.28 (td, J=8.0, 1.7 Hz, 1H), 7.24 (d, J=1.7 Hz, 1H), 7.19 (dd, J=8.0, 1.2 Hz, 1H), 7.11 (dd, J=7.7, 4.6 Hz, 1H), 7.02 (td, J=7.5, 1.2 Hz, 1H); LC/MS [M+H]: 235.

1. temperatureAfter cooling to room temperature the solvent
2. customwas removed under reduced pressure
3. additionThe resulting crude product was diluted with acetone
4. filtrationfiltered by suction