反应详情

温度

0 °C

The product from step (c) (20.0 g, 68.2 mmol) was dissolved in dichloromethane (200 mL) and cooled to 0° C. Boron trifluoride diethyl etherate (10.4 mL, 82.0 mmol) was added via syringe and the mixture was warmed to room temperature to give a thick suspension. The suspension was heated at 45° C. (oil bath) and a solution of bromine (11.5 g, 72.0 mmol) in dichloromethane (100 mL) was added over 40 min. The mixture was kept at 45° C. for an additional 15 min and then cooled to room temperature. The mixture was concentrated under reduced pressure and then triturated with 10% aqueous sodium carbonate (200 mL) for 1 hour. The solids were collected on a Buchner funnel, washed with water (4×100 mL) and dried under reduced pressure. The product of two runs was combined for purification. The crude product (52 g) was triturated with 50% methanol in chloroform (500 mL) for 1 hour. The product was collected on a Buchner funnel and washed with 50% methanol in chloroform (2×50 mL) and methanol (2×50 mL). The solid was dried under reduced pressure to give the title compound (34.1 g) as a powder.

1. temperaturethe mixture was warmed to room temperature
2. customto give a thick suspension
3. temperatureThe suspension was heated at 45° C. (oil bath)
4. temperaturecooled to room temperature
5. concentrationThe mixture was concentrated under reduced pressure
6. customtriturated with 10% aqueous sodium carbonate (200 mL) for 1 hour
7. customThe solids were collected on a Buchner funnel
8. washwashed with water (4×100 mL)
9. customdried under reduced pressure
10. customThe product of two runs was combined for purification
11. customThe crude product (52 g) was triturated with 50% methanol in chloroform (500 mL) for 1 hour
12. customThe product was collected on a Buchner funnel
13. washwashed with 50% methanol in chloroform (2×50 mL) and methanol (2×50 mL)
14. customThe solid was dried under reduced pressure