反应详情

A solution of tert-butyl 6-methyl-8-(2-oxo-4-(6-(trifluoromethyl)pyridin-3-yl)pyridin-1(2H)-yl)3,4,5,6-tetrahydroazepino[4,3-b]indole-2(1H)-carboxylate (67 mg, 0.13 mmol) in 1.25 M HCl in MeOH (16 mL) was stirred at ambient temperature for 18 h. The mixture was concentrated to dryness under reduced pressure and diluted with MeOH (2.0 mL) and Et2O (25 mL). The resulting solids were collected by filtration and dried to yield the title compound (42 mg, 70%) as a yellow powder: mp 274-280° C. decomp; 1H NMR (500 MHz, DMSO-d6) δ 9.50 (s, 2H), 9.20 (d, J=2.0 Hz, 1H), 8.50 (dd, J=8.0, 2.0 Hz, 1H), 8.05 (d, J=8.0 Hz, 1H), 7.86 (d, J=7.0 Hz, 1H), 7.69 (d, J=8.5 Hz, 1H), 7.59 (d, J=1.5 Hz, 1H), 7.09 (dd, J=8.5, 2.0 Hz, 1H), 7.00 (d, J=2.0 Hz, 1H), 6.80 (d, J=7.5, 2.0 Hz, 1H), 4.42-4.41 (m, 2H), 3.73 (s, 3H), 3.43-3.41 (m, 2H), 3.11 (t, J=6.0 Hz, 2H), 2.10-2.08 (m, 2H); ESI MS m/z 439 [M+H]+; HPLC (Method A) 99.0% (AUC), tR=13.7 min.

1. concentrationThe mixture was concentrated to dryness under reduced pressure
2. additiondiluted with MeOH (2.0 mL) and Et2O (25 mL)
3. filtrationThe resulting solids were collected by filtration
4. customdried