反应详情

To the title compound of step 2 (2.00 g, 7.69 mmol, 1.00 Eq) in MeOH (50 mL)/EtOH (50 mL)/DMF (10 mL) was added Pd—C (10%, 0.2 g) under N2. The suspension was purged with H2 three times and hydrogenated under a balloon for 5 h. The catalyst was removed by fitration, and anhydrous HCl in methanol (10 mL, 1.25 M) was added. Concentration left a residue which was treated a second time with HCl in methanol. Evaporation of the volatile components and triturtion with DCM (30 mL)/hexane (30 mL) gave the title compound (1.29 g, 7.30 mmol, yield: 95%) as a pink HCl salt after drying. 1H NMR: (DMSO-d6, 400 MHz) δ: 9.45-8.02 (br, 3H), 7.64 (d, J=7.6 Hz, 1H), 3.27 (d, J=7.6 Hz, 1H), 3.43 (s, 3H). LCMS: 163.0 (M+Na)+

1. customThe suspension was purged with H2 three times and hydrogenated under a balloon for 5 h
2. customThe catalyst was removed by fitration, and anhydrous HCl in methanol (10 mL, 1.25 M)
3. additionwas added
4. concentrationConcentration
5. waitleft a residue which
6. additionwas treated a second time with HCl in methanol
7. customEvaporation of the volatile components and triturtion with DCM (30 mL)/hexane (30 mL)