Phosphorus tribromide → 1,2,3,4,5,6,7,8-Octafluoro-9-(pentafluorophenyl)-fluorene
反応式
[F:1][C:2]1[C:14]2[C:13](O)([C:15]3[C:20]([F:21])=[C:19]([F:22])[C:18]([F:23])=[C:17]([F:24])[C:16]=3[F:25])[C:12]3[C:7](=[C:8]([F:30])[C:9]([F:29])=[C:10]([F:28])[C:11]=3[F:27])[C:6]=2[C:5]([F:31])=[C:4]([F:32])[C:3]=1[F:33].P(Br)(Br)Br>>[F:1][C:2]1[C:14]2[CH:13]([C:15]3[C:16]([F:25])=[C:17]([F:24])[C:18]([F:23])=[C:19]([F:22])[C:20]=3[F:21])[C:12]3[C:7](=[C:8]([F:30])[C:9]([F:29])=[C:10]([F:28])[C:11]=3[F:27])[C:6]=2[C:5]([F:31])=[C:4]([F:32])[C:3]=1[F:33]参加物
3
実験手順
4.5 g (0.009 moles) of 1,2,3,4,5,6,7,8-octafluoro-9-hydroxy-9-(pentafluorophenyl)fluorene thus prepared, are added to 25 ml (0.26 moles) of PBr3 and heated to 1100C for 30 minutes in an inert atmosphere. The reaction mass is hydrolyzed in ice, extracted with ethyl ether, the extract is washed with an aqueous solution (10%) of NaHCO3, dried on sodium sulfate, filtered and dried. The residue is purified by chromatography on a silica gel column (eluant: petroleum ether/methylene chloride, 98/2), obtaining, after evaporation of the pure fractions, 3.61 g of white crystalline product corresponding to the desired product having formula (VI) (yield 84%) (characterization by means of 1H-NMR and