tert-Butyl [(4-fluoro-3-nitrophenyl)methyl]carbamate → tert-Butyl [(3-amino-4-fluorophenyl)methyl]carbamate

HRID 2366748ノート

反応式

HRID 2366748 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][NH:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:4][C:3]=1[N+:17]([O-])=O>CO.[C].[Pd]>[NH2:17][C:3]1[CH:4]=[C:5]([CH2:8][NH:9][C:10](=[O:16])[O:11][C:12]([CH3:14])([CH3:13])[CH3:15])[CH:6]=[CH:7][C:2]=1[F:1]

参加物

4

反応物 1

HCID 53420783tert-Butyl [(4-fluoro-3-nitrophenyl)methyl]carbamate

生成物 1

HCID 53439222tert-Butyl [(3-amino-4-fluorophenyl)methyl]carbamate収率 99%

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 tert-butyl (4-fluoro-3-nitrophenyl)methylcarbamate (1.0 g, 3.70 mmol) in methanol (4 mL) was added 10% palladium-carbon (150 mg), and the mixture was stirred at room temperature under a hydrogen atmosphere (1 atm) for 18 hr. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (ethyl acetate), and the obtained solution was concentrated under reduced pressure to give the title compound (0.88 g, 99%) as a brown oil.

後処理

  1. filtrationThe insoluble material was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customThe obtained residue was purified by silica gel column chromatography (ethyl acetate)
  4. concentrationthe obtained solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-fbd03f4d51af4a36990ed0dbf1abd520
出典データセット
uspto-grants-2014_04
特許番号
US08697874B2

反応ノート

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