反应详情

A solution of 4-[(2,4-dimethoxybenzyl)amino]-2-methyl-1,2-dihydro-3H-pyrrolo[3,4-c]pyridin-3-one (1.8 g, 5.7 mmol) in 37% HCl (7.0 mL) was stirred at rt for 16 hours. The reaction mixture was neutralized with NaOH and extracted with EtOAc (15 mL). The organic layer was washed with water (10 mL), washed with brine (10 mL), dried over Na2SO4, filtered, and concentrated under reduced pressure to yield a red solid. The crude material was purified by silica gel chromatography on the combi-flash Rf system using DCM/MeOH (100:0→95:5) as eluent. The fractions containing product were combined and concentrated under reduced pressure to yield an orange solid, (319 mg, 34%). 1H NMR (DMSO-d6, 400 MHz): δ=2.99 (s, 3 H), 4.37 (s, 2 H), 6.54 (br. s., 2 H), 6.73 (d, J=5.05 Hz, 1 H), 8.04 (d, J=5.05 Hz, 1 H). MS (ES+): m/z 164.07 [MH+] (TOF, polar).

1. extractionextracted with EtOAc (15 mL)
2. washThe organic layer was washed with water (10 mL)
3. washwashed with brine (10 mL)
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customto yield a red solid
8. customThe crude material was purified by silica gel chromatography on the combi-flash Rf system
9. additionThe fractions containing product
10. concentrationconcentrated under reduced pressure
11. customto yield an orange solid, (319 mg, 34%)