反应详情

To a solution of 2-{2-[2-(3-methoxyphenyl)-1-pyrrolidinyl]ethyl}-1H-isoindole-1,3(2H)dione (1.0 g), in dry chloroform (40 ml) was added boron tribromide (99%, 1.3 ml) at -10° C., under nitrogen. The reaction mixture was stirred for 10 mins in a cooling bath and 20 mins at ambient temperature. Crushed ice was added followed by 5:1-chloroform/2-propanol (10 ml). The layers were separated, and the aqueous phase was extracted with 5:1-chloroform/2-propanol (2 times). The combined organic extracts were washed with saturated sodium bicarbonate solution, dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated to give 0.89 g (93%) of product, mp 172°-175° C.

1. additionCrushed ice was added
2. customThe layers were separated
3. extractionthe aqueous phase was extracted with 5
4. washThe combined organic extracts were washed with saturated sodium bicarbonate solution
5. dry with materialdried over anhydrous sodium sulfate
6. filtrationfiltered
7. concentrationthe filtrate was concentrated