N-tert-butyl-2-nitro-4-(trifluoromethyl)aniline → HCID 18509812、化合物

HRID 2390498ノート

反応式

HRID 2390498 の反応式
[C:1]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([F:15])([F:14])[F:13])=[CH:8][C:7]=1[N+:16]([O-])=O)([CH3:4])([CH3:3])[CH3:2]>[Pd].C(OCC)(=O)C>[C:1]([NH:5][C:6]1[C:7]([NH2:16])=[CH:8][C:9]([C:12]([F:14])([F:15])[F:13])=[CH:10][CH:11]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 1

HCID 2736447N-tert-butyl-2-nitro-4-(trifluoromethyl)aniline

生成物 1

HCID 18509812HCID 18509812、化合物収率 103.7%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 5.25 g of N-tert-butyl-2-nitro-4-trifluoromethylaniline, 20 ml of ethyl acetate and 5% palladium charcoal was stirred for 9 hours at room temperature under a hydrogen atmosphere of about 1 atm. The reaction mixture was filtrated through Celite (registered trademark). The filtrate was washed with water, dried over sodium sulfate, then, concentrated under reduced pressure to obtain a residue. The resultant residue was subjected to silica gel chromatography to obtain 4.82 g of N1-tert-butyl-4-trifluoromethylbenzene-1,2-diamine.

後処理

  1. filtrationThe reaction mixture was filtrated through Celite (registered trademark)
  2. washThe filtrate was washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customto obtain a residue

出典と根拠

ORDレコード
ord-6485d872bbb344398211469e11bbc72a
出典データセット
uspto-grants-2012_09
特許番号
US08273764B2

反応ノート

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