反应详情

A solution of 1-(9-methyl-5,7,8,9-tetrahydro-6H-pyrido[3′,4′:4,5]pyrrolo[2,3-b]pyridin-2-yl)-4-((6-(trifluoromethyl)pyridin-3-yl)methoxy)pyridin-2(1H)-one (0.27 g, 0.59 mmol) in MeOH (2.0 mL) was treated with 1.25 M HCl in MeOH (0.47 mL, 0.59 mmol), and the resulting suspension was stirred at ambient temperature for 6 h. The suspension was diluted with Et2O, and the resulting solids were collected by filtration. The filtrate was concentrated, and the resulting residue was dissolved in CH2Cl2 (0.5 mL) and diluted with Et2O (50 mL). The resulting solids were collected by filtration. The solids from both batches were combined in Et2O and the resulting slurry was concentrated to dryness to provide the title compound (0.23 g, 78%) as an off-white powder: 280-278° C. decomp.; 1H NMR (500 MHz, DMSO-d6) δ 8.89 (d, J=1.0 Hz, 1H), 8.19 (d, J=8.0, 1.5 Hz, 1H), 8.17-7.80 (m, 4H), 7.33 (d, J=8.5 Hz, 1H), 6.21 (dd, J=7.5, 2.5 Hz, 1H), 6.04 (d, J=2.5 Hz, 1H), 5.36 (s, 2H), 4.22 (s, 2H), 3.69 (s, 3H), 3.41 (t, J=6.0 Hz, 2H), 3.01 (t, J=5.5 Hz, 2H); ESI MS m/z 456 [M+H]; HPLC (Method A)>99% (AUC), tR=13.4 min.

1. filtrationthe resulting solids were collected by filtration
2. concentrationThe filtrate was concentrated
3. dissolutionthe resulting residue was dissolved in CH2Cl2 (0.5 mL)
4. additiondiluted with Et2O (50 mL)
5. filtrationThe resulting solids were collected by filtration
6. concentrationthe resulting slurry was concentrated to dryness