反应详情

温度

-78 °C

2-(3-Methoxyphenyl)benzoic acid from Step B (6.53 g, 28.6 mmol) was dissolved in dry CH2Cl2 (100 mL) under argon and cooled to −78° C. Boron tribromide (62.9 mL of a 1.0 M solution in CH2Cl2, 62.9 mmol) was added dropwise and the solution was stirred overnight and allowed to warm slowly to ambient temperature. The resulting mixture was cooled in an ice bath and quenched carefully with water (200 mL), then extracted with CH2Cl2 (3×250 mL). The combined organic extracts were dried over Na2SO4, filtered, and concentrated under reduced pressure to give the titled product which was sufficiently pure for use in the next step.

1. temperatureto warm slowly to ambient temperature
2. temperatureThe resulting mixture was cooled in an ice bath
3. customquenched carefully with water (200 mL)
4. extractionextracted with CH2Cl2 (3×250 mL)
5. dry with materialThe combined organic extracts were dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure