Tetrahydrofuran → HCID 66810289、化合物

HRID 455244ノート

反応式

HRID 455244 の反応式
[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]

参加物

5

反応物 2

HCID 8028TetrahydrofuranHCID 66810464HCID 66810464、化合物

生成物 1

HCID 66810289HCID 66810289、化合物収率 87.7%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e54c6bc4cb7f4a46ba3ab8bf57b8cf36
出典データセット
uspto-grants-2013_07
特許番号
US08497274B2

反応ノート

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