反应详情

温度

10 °C

A 4-L RB flask, equipped a magnetic stirring bar was charged with pyrrolidine (363 g, 426 mL, 5.1 mol) and acetonitrile (2750 mL). The mixture was cooled with an ice bath to 10° C., then solid 4-bromo-2-fluorobenzylbromide (MATRIX, Cat. #: 1707, 375 g, 1.4 mol) was added in 6 portions, keeping temperature below 20° C. The mixture was stirred at RT for 4 h. The solvent was removed under vacuum. Then 2 L of sat. Na2CO3 aq. and 500 mL of water was added, and the mixture was extracted with DCM (3×700 mL). The extract was dried over Na2SO4 and evaporated. The resulting light yellow oil was distilled under vacuum (˜1 mm, bp. 125° C.) to give 324.5 g (90%) of the product as a colorless oil. LCMS (M+H): 258.5.

1. customtemperature below 20° C
2. customThe solvent was removed under vacuum
3. additionThen 2 L of sat. Na2CO3 aq. and 500 mL of water was added
4. extractionthe mixture was extracted with DCM (3×700 mL)
5. dry with materialThe extract was dried over Na2SO4
6. customevaporated
7. distillationThe resulting light yellow oil was distilled under vacuum (˜1 mm, bp. 125° C.)