反应详情

A mixture of 5a (56.0 g, 193 mmol), p-TSA (36.0 g, 193 mmol) and phenol (25.0 g, 251 mmol) was heated to 95 for 1 h. After cooling to room temperature, the reaction mixture was partitioned between DCM and water. The separated organic phase was washed with water, three times with saturated aqueous sodium bicarbonate, brine, dried (MgSO4) and concentrated in vacuo to afford the title compound 5b. This was used without further purification in the subsequent step.

1. temperaturewas heated to 95 for 1 h
2. customthe reaction mixture was partitioned between DCM and water
3. washThe separated organic phase was washed with water, three times with saturated aqueous sodium bicarbonate, brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated in vacuo