反应详情

To a solution of compound 2A (2 g, 11 mmol) in AcOH (15 mL) cooled at 0° C. was added a solution of bromine (1.69 mL, 33 mmol) in AcOH (1.2 mL) slowly so that the reaction temperature was maintained below 17° C. After addition, the reaction mixture was stirred at rt until all the starting material was consumed (˜4 h). The reaction mixture was then poured into ice/water and the resulting suspension filtered. The collected solid was washed with H2O until the filtrate pH=6-7, and dried in a vacuum oven at 50° C. overnight to yield compound 2B (2.7 g) as an off-white solid.

1. temperaturewas maintained below 17° C
2. additionAfter addition
3. customwas consumed (˜4 h)
4. additionThe reaction mixture was then poured into ice/water
5. filtrationthe resulting suspension filtered
6. washThe collected solid was washed with H2O until the filtrate pH=6-7
7. customdried in a vacuum oven at 50° C. overnight