Tetrahydrofuran → HCID 66810289, 화합물

HRID 1097534노트

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HRID 1097534 반응식
[F:1][C:2]1[CH:21]=[CH:20][C:5]([O:6][C:7]2[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[CH:13][C:8]=2[C:9]([O:11][CH3:12])=[O:10])=[CH:4][C:3]=1[NH:22][C:23](=[O:35])[CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[C:27]([C:31]([F:34])([F:33])[F:32])[CH:26]=1.O1CCCC1>CO.[C].[Pd]>[NH2:17][C:14]1[CH:15]=[CH:16][C:7]([O:6][C:5]2[CH:20]=[CH:21][C:2]([F:1])=[C:3]([NH:22][C:23](=[O:35])[CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[C:27]([C:31]([F:34])([F:32])[F:33])[CH:26]=3)[CH:4]=2)=[C:8]([CH:13]=1)[C:9]([O:11][CH3:12])=[O:10]

참가 물질

5

반응물 2

HCID 8028TetrahydrofuranHCID 66810464HCID 66810464, 화합물

생성물 1

HCID 66810289HCID 66810289, 화합물수율 87.7%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

To a solution of methyl 2-[4-fluoro-3-({[3-(trifluoromethyl)phenyl]acetyl}amino)phenoxy]-5-nitrobenzoate (3.75 g, 7.62 mmol) in methanol (40 mL)/tetrahydrofuran (8 mL) solution was added 10% palladium-carbon (400 mg), and the mixture was stirred at room temperature for 6 hr under a hydrogen atmosphere (1 atm). Insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by basic silica gel column chromatography (ethyl acetate/n-hexane=30/70→80/20), and the fraction containing the object product was concentrated under reduced pressure to give the title compound (3.09 g, 87%) as a yellow oil.

후처리

  1. filtrationInsoluble material was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe obtained residue was purified by basic silica gel column chromatography (ethyl acetate/n-hexane=30/70→80/20)
  4. additionthe fraction containing the object product
  5. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-94dc8fb78e3a452a9853cd460e9f1cd4
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143258B2

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