反应详情

3-(Amino methyl)-4-ethyl-6-methylpyridin-2(1H)-one, (5.6 g, 33 mmol) was suspended in DCM (560 mL) and the insoluble contents/particles were filtered. The filtrate was concentrated and dried. The residue was dissolved in DCM (10 mL) and 4 M HCl in 1,4-dioxane (16 mL, 66 mmol) was added at 0° C. and stirred for 10 min, at which time the reaction mixture was concentrated under high-vacuum and dried. The resulting crude solid was triturated with hexane (150 mL) and filtered. The solid was dried under vacuum. Collected 3-(amino methyl)-4-ethyl-6-methylpyridin-2(1H)-one hydrochloride (5.9 g, 86%). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.082-1.120 (t, 3H, J=7.6 Hz), 2.179 (s, 3H), 2.503-2.544 (m, 2H), 3.785-3.798 (d, 2H, J=5.2 Hz), 6.024 (s, 1H), 7.985 (broad s, 2H), 11.858 (broad s, 1H). MS(ES) [M+H]+ 167.2.

1. filtrationthe insoluble contents/particles were filtered
2. concentrationThe filtrate was concentrated
3. customdried
4. dissolutionThe residue was dissolved in DCM (10 mL)
5. concentrationwas concentrated under high-vacuum
6. customdried
7. customThe resulting crude solid was triturated with hexane (150 mL)
8. filtrationfiltered
9. customThe solid was dried under vacuum