反应详情

A mixture of 6-nitro-N-[(3S)-tetrahydro-2H-pyran-3-yl]thieno[3,2-b]pyridin-7-amine (30 mg, 0.1 mmol), iron (18 mg, 0.32 mmol) and ammonium chloride (29 mg, 0.54 mmol) in ethanol (0.8 mL)/water (0.3 mL) was heated at reflux for 4 h. The resulting mixture was filtered. The filtrate was diluted with EtOAc, washed with sat. NaHCO3 solution, dried over MgSO4, and concentrated. The residue was purified on silica gel (eluting with 0 to 5% MeOH in dichloromethane) to give the desired product. LCMS calculated for C12H16N3OS (M+H)+: m/z=250.1. Found: 250.0.

1. temperaturewas heated
2. temperatureat reflux for 4 h
3. filtrationThe resulting mixture was filtered
4. additionThe filtrate was diluted with EtOAc
5. washwashed with sat. NaHCO3 solution
6. dry with materialdried over MgSO4
7. concentrationconcentrated
8. customThe residue was purified on silica gel (eluting with 0 to 5% MeOH in dichloromethane)