反应详情

To a stirring solution of 39d (0.389 g, 1 mmol) in dichloromethane (15 ml) under Ar was added boron tribromide in dichloromethane (1.0M, 5.0 ml, 5 mmol, 4.9 equ). The mixture was then stirred for 18 hours. Methanol (5 ml) was then added. The reaction was heated to reflux for 2 hours, then concentrated in vacuo to give a brown solid. Water (25 ml) was added and the mixture sonicated then extracted into ethyl acetate (3×). The organic layer was washed with brine then dried (MgSO4) and concentrated in vacuo to give 9d (0.302 g, 77%) as a brown solid.

1. temperatureThe reaction was heated
2. temperatureto reflux for 2 hours
3. concentrationconcentrated in vacuo
4. customto give a brown solid
5. customthe mixture sonicated
6. extractionthen extracted into ethyl acetate (3×)
7. washThe organic layer was washed with brine
8. dry with materialthen dried (MgSO4)
9. concentrationconcentrated in vacuo