5-benzyl-10-fluoro-5H-dibenz[b,f]azepine → 10-fluoro-5H-dibenz[b,f]azepine

HRID 616885

반응식

HRID 616885 반응식
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

참가 물질

5

반응물 2

HCID 203664075-benzyl-10-fluoro-5H-dibenz[b,f]azepineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 2036640810-fluoro-5H-dibenz[b,f]azepine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

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.

후처리

  1. custom(app. 15 hours)
  2. filtrationThe catalyst is filtered off
  3. concentrationthe filtrate is concentrated in vacuo
  4. 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
  5. concentrationconcentrated by rotary evaporation
  6. customthe residue is crystallised from ether/hexane

출처 및 근거

ORD 기록
ord-ade755ed64bf4eb488dae0d3cae1edfe
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04076812

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