反应详情

Methylenecyclobutane (5.00 g, 70.5 mmol) and zinc dust (13.8 g, 211 mmol) were suspended in dry Et2O (200 mL) in a 3 necked round bottomed flask having an addition funnel and reflux condenser and placed in a sonic bath at 25° C. The system was sonicated and 2,2,2-trichloroacetyl chloride (10.282 mL, 91.607 mmol) (as a solution in 50 mL dry Et2O) added drop-wise, during which time the reaction became warm and the Et2O began refluxing). The sonication was continued for 4 hours. The reaction mixture was filtered through a pad of Celite® and the organic layer was washed sequentially with NH4Cl, NaHCO3 and brine. The organic layer was dried (MgSO4), filtered and concentrated under reduced pressure to afford the crude material, which was in the next step without purification.

1. temperaturereflux condenser
2. customplaced in a sonic bath at 25° C
3. customThe system was sonicated
4. temperatureduring which time the reaction became warm
5. customThe sonication
6. filtrationThe reaction mixture was filtered through a pad of Celite®
7. washthe organic layer was washed sequentially with NH4Cl, NaHCO3 and brine
8. dry with materialThe organic layer was dried (MgSO4)
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure