反应详情

To a solution of 45 (1.1 g, 0.717 mmol) in MeOH (30 mL) and water (10 mL) was added ammonium chloride (211 mg, 3.95 mmol) and zinc (1.61 g, 17.76 mmol) and the reaction mixture was heated to reflux for 24 hours. The reaction mixture was cooled to RT then concentrated to dryness. The residue was partitioned between DCM and water and the organic phase was collected, dried over Na2SO4, filtered and concentrated to afford the title compound 46 (1.04 g, 100% yield), which was used crude in the next step with no additional purification. MS (m/z): 528.1 (M+H).

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 24 hours
3. concentrationthen concentrated to dryness
4. customThe residue was partitioned between DCM and water
5. customthe organic phase was collected
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated