反应详情

温度

0 °C

To a solution of 3-(4-bromophenyl)-propionic acid (9.16 g, 40 mmol) in THF (150 mL) at 0° C. was added LiAlH4 (1.4 g, 36 mmol) in portionwise. When the addition was completed, the reaction mixture was heated and stirred under reflux for additional 5 hours. The reaction mixture was cooled to 0° C. and 2 N—HCl (50 mL) added dropwise. The reaction mixture was extracted with EtOAc and washed with water (×3). The combined organic extract was dried over anhydrous MgSO4, filtered and concentrated in vacuo, which afforded the subtitle compound (i) as an oil (8 g).

1. additionWhen the addition
2. temperaturethe reaction mixture was heated
3. temperatureunder reflux for additional 5 hours
4. extractionThe reaction mixture was extracted with EtOAc
5. washwashed with water (×3)
6. extractionThe combined organic extract
7. dry with materialwas dried over anhydrous MgSO4
8. filtrationfiltered
9. concentrationconcentrated in vacuo, which