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1-(4'-Hydroxymethyl-4,6-dinitro-biphenyl-3-yl)-propan-2-one → [4-(2-methyl-6-nitro-1H-indol-5-yl)-phenyl]-methanol

HRID 1773537
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HRID 1773537 반응식
[OH:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][C:12]([N+:18]([O-])=O)=[C:11]([CH2:21][C:22](=O)[CH3:23])[CH:10]=2)=[CH:5][CH:4]=1>[Pd].C(OCC)(=O)C>[CH3:23][C:22]1[NH:18][C:12]2[C:11]([CH:21]=1)=[CH:10][C:9]([C:6]1[CH:7]=[CH:8][C:3]([CH2:2][OH:1])=[CH:4][CH:5]=1)=[C:14]([N+:15]([O-:17])=[O:16])[CH:13]=2.[OH:16][NH:15][C:14]1[CH:13]=[C:12]2[C:11]([CH:21]=[C:22]([CH3:23])[NH:18]2)=[CH:10][C:9]=1[C:6]1[CH:7]=[CH:8][C:3]([CH2:2][OH:1])=[CH:4][CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 580561251-(4'-Hydroxymethyl-4,6-dinitro-biphenyl-3-yl)-propan-2-one

생성물 2

HCID 66665074[4-(2-methyl-6-nitro-1H-indol-5-yl)-phenyl]-methanolHCID 86661370(4-(6-(Hydroxyamino)-2-methyl-1h-indol-5-yl)phenyl)methanol

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 1-(4′-hydroxymethyl-4,6-dinitro-biphenyl-3-yl)-propan-2-one (200 mg) and palladium on carbon (10%, 80 mg) in ethyl acetate was shaken in a Parr apparatus under hydrogen atmosphere (50 PSI) overnight. The reaction mixture was then filtered on a CELITE™ pad, the filtrate was evaporated under reduced pressure and the crude residue was purified by flash chromatography to afford [4-(2-methyl-6-nitro-1H-indol-5-yl)-phenyl]-methanol and [4-(6-hydroxyamino-2-methyl-1H-indol-5-yl)-phenyl]-methanol. The two products were combined and dissolved in dichloromethane (5 mL). Zinc dust (a large excess) and glacial acetic acid (1 mL) were added and the resulting mixture was heated at 70° C. for 30 minutes. The reaction mixture was then filtered on a CELITE™ pad, the filter cake was washed with ethyl acetate. The filtrate was washed with brine, dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure. The crude residue was purified by flash chromatography (MeOH/DCM, 5/95) to give 55 mg of [4-(6-amino-2-methyl-1H-indol-5-yl)-phenyl]-methanol. MS=253 [M+H]+.

후처리

  1. filtrationThe reaction mixture was then filtered on a CELITE™ pad
  2. customthe filtrate was evaporated under reduced pressure
  3. customthe crude residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-dae74c01603048b2b7b3818ba5595619
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09255110B2

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