反应详情

A 2 L 24/40 three necked round-bottom flask equipped with a mechanical stirrer, a reflux condenser and a stopper, was charged with 15.427 g (72 mmol) of 4-methyl-2'-nitro[1,1'-biphenyl], 1.2 L of carbon tetrachloride, 14.164 g (80 mmol) of N-bromosuccinimide, and 0.50 g of 2,2'-azobis(2-methylpropionitrile). The stirred reaction mixture was refluxed under a nitrogen atmosphere for 4 hours, then cooled to room temperature and filtered. The filtrate was evaporated in vacuo and the residual oil was purified on a silica gel flash chromatography column eluted with 10% ethyl acetate-hexane. Evaporation of the pure fractions afforded the product as a yellow crystalline solid (7.83 g, 37%) which had: mp 109°-110° C.

1. customThe stirred reaction mixture
2. temperaturewas refluxed under a nitrogen atmosphere for 4 hours
3. filtrationfiltered
4. customThe filtrate was evaporated in vacuo
5. customthe residual oil was purified on a silica gel flash chromatography column
6. washeluted with 10% ethyl acetate-hexane
7. customEvaporation of the pure fractions