反应详情

A solution of m-chlorotoluene (12.66 g, 0.100 mol) and 1,2-dibromoethane (0.5 ml) in THF (20 ml) was added to magnesium turnings (2.67 g, 0.110 mol). The mixture was heated under reflux for 4 h, after which the heating bath was removed and trimethylchlorosilane (11.08 g, 0.102 mol) was added so that gentle reflux was maintained. The mixture was stirred for another 0.5 h and 5% NaHCO3 (100 ml) was then added. The resulting mixture was extracted with CH2Cl2 (3×50 ml), the organic phase was washed with brine and dried (MgSO4). Filtration and evaporation provided 15.05g (92%) of 36 as a pale yellow liquid. Spectroscopic data were identical to those previously reported in the literature.40

1. temperatureThe mixture was heated
2. temperatureunder reflux for 4 h
3. customafter which the heating bath was removed
4. temperaturethat gentle reflux
5. temperaturewas maintained
6. extractionThe resulting mixture was extracted with CH2Cl2 (3×50 ml)
7. washthe organic phase was washed with brine
8. dry with materialdried (MgSO4)
9. filtrationFiltration and evaporation