反应详情

To a stirred and ice-cooled mixture of Compound 3 (10.0 g, 27.1 mmol), 3.0 M NaOH aq. (36.1 ml, 108.4 mmol) and tert-BuOH (15.0 ml) was added (tert-BuOCO)2O (Boc2O, 7.39 g, 33.8 mmol). After stirring at room temperature overnight, the mixture was extracted with AcOEt (x3). The combined AcOEt extracts were washed with sat. NaHCO3 and brine, dried over Na2SO4, and concentrated to give Compound 4 (11.3 g, quant.) as a pale yellow syrup.

1. temperatureice-cooled
2. stirringAfter stirring at room temperature overnight
3. extractionthe mixture was extracted with AcOEt (x3)
4. washThe combined AcOEt extracts were washed with sat. NaHCO3 and brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated