反应详情

A mixture of O-methylhydroxylamine hydrochloride (535 mg, 6.40 mmol), 2-amino-4-(2-methyl-1,3-dioxolan-2-yl)phenol D130 (250 mg, 1.28 mmol) and potassium carbonate (442 mg, 3.20 mmol) in ethanol (10 mL) was heated to reflux for 2 hr. The mixture was cooled to rt and concentrated to dryness under vacuum and the residue partitioned between DCM and water. The organic phase was separated washed with brine, dried (MgSO4) and concentrated to dryness in vacuo. The residue was purified using silica gel chromatography eluting with 0 to 10% MeOH in DCM. The title product was isolated as a pale brown solid, 224 mg, 97%.

1. temperaturewas heated
2. temperatureto reflux for 2 hr
3. concentrationconcentrated to dryness under vacuum
4. customthe residue partitioned between DCM and water
5. customThe organic phase was separated
6. washwashed with brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated to dryness in vacuo
9. customThe residue was purified
10. washeluting with 0 to 10% MeOH in DCM