反应详情

温度

40 °C

To a mixture of 4-hydroxy-3-methoxybenzonitrile (2.6 g, 17.6 mmol), ethyl [(1S)-5-(3-bromopropoxy)-2,3-dihydro-1H-inden-1-yl]acetate (Example 45) (6 g, 17.6 mmol), and Cs2CO3 (6.9 g, 21.1 mmol) in DMF (30 mL) was added water (15 drops). The reaction mixture was stirred at 40° C. for 16 h and concentrated under reduced pressure. The residue was diluted with water and extracted with EtOAc (2×). The combined organic phases were dried over MgSO4, filtered, and concentrated under reduced pressure. Recrystallization from MeOH (5 mL) gave 4.9 g (68%) of the title compound as an off-white solid. LC-MS: RT=3.59 min; (M+H)+ 410.0.

1. concentrationconcentrated under reduced pressure
2. additionThe residue was diluted with water
3. extractionextracted with EtOAc (2×)
4. dry with materialThe combined organic phases were dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customRecrystallization from MeOH (5 mL)