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

HRID 1256623ノート

反応式

HRID 1256623 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-5075bff341504c0e81c816b14e578837
出典データセット
uspto-grants-2013_06
特許番号
US08461181B2

反応ノート

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