反応式
C([N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[C:12]([F:19])=[CH:11][C:10]2[CH:20]=[CH:21][CH:22]=[CH:23][C:9]1=2)C1C=CC=CC=1.[H][H]>CO.[Pd]>[F:19][C:12]1[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[NH:8][C:9]2[CH:23]=[CH:22][CH:21]=[CH:20][C:10]=2[CH:11]=1参加物
5
実験手順
A solution of 6.03 g (0.02 mole) of 5-benzyl-10-fluoro-5H-dibenz[b,f]azepine in 100 ml of methanol is hydrogenated at 25° C in the presence of 0.6 of palladium on charcoal catalyst (5% Pd) until the uptake of hydrogen has ceased (app. 15 hours). The catalyst is filtered off and the filtrate is concentrated in vacuo. The residual colourless oil is chromatographed over 50 times the amount of silica gel (particle size: 0.063-0.2 mm) with benzene/petroleum ether (1:1) as eluant. The homogeneous fractions are combined, concentrated by rotary evaporation and the residue is crystallised from ether/hexane to yield 10-fluoro-5H-dibenz[b,f]azepine of m.p. 69°-72° C.
後処理
- custom(app. 15 hours)
- filtrationThe catalyst is filtered off
- concentrationthe filtrate is concentrated in vacuo
- customThe residual colourless oil is chromatographed over 50 times the amount of silica gel (particle size: 0.063-0.2 mm) with benzene/petroleum ether (1:1) as eluant
- concentrationconcentrated by rotary evaporation
- customthe residue is crystallised from ether/hexane
出典と根拠
- ORDレコード
- ord-ade755ed64bf4eb488dae0d3cae1edfe
- 出典データセット
- uspto-grants-1978_02
- 特許番号
- US04076812
関連ノート
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