反应详情

温度

5 °C

To a solution of 47 (2.0 g, 4.5 mmol) in IPAC (20 mL) was added p-toluenesulfonic acid monohydrate (1.3 g, 6.8 mmol). The mixture was aged at 55° C. for 4 h. After the reaction was complete, the slurry was cooled in an ice bath to 5° C. and a solution of potassium carbonate (1.9 g, 13.6 mmol) in H2O (10 mL) was added. The aqueous layer (pH=10) was separated and the organic layer was washed with saturated aqueous NaHCO3, water and brine, in turns, and dried over Na2SO4. Concentration afforded 48 (1.3 g, 86% yield) as a 4:1 mixture of diastereomers.

1. customThe aqueous layer (pH=10) was separated
2. washthe organic layer was washed with saturated aqueous NaHCO3, water and brine, in turns
3. dry with materialdried over Na2SO4
4. concentrationConcentration