反应详情

温度

-10 °C

1-(4-Hydroxy-3-trifluoromethylphenyl)ethanone (5 g) was initially charged in acetonitrile (150 ml) at RT while stirring, and cooled to −10° C. At this temperature, N-bromosuccinimide (4.5 g, dissolved in 100 ml of acetonitrile) was added dropwise. Then the cooling bath was removed and the mixture was stirred for a further 5 h. After standing overnight, ¾ of the solvent was drawn off and the residue was admixed with n-heptane/water. The organic phase was removed and washed once with 5% sodium thiosulfate solution and once with water. The precipitate formed was filtered off with suction, washed and dried. 6.9 g of the title compound were obtained in sufficient purity. LC-MS rt: 1.35 min [M+H]+: 283.0 (met. a)

1. customThen the cooling bath was removed
2. stirringthe mixture was stirred for a further 5 h
3. customThe organic phase was removed
4. washwashed once with 5% sodium thiosulfate solution and once with water
5. customThe precipitate formed
6. filtrationwas filtered off with suction
7. washwashed
8. customdried