1-tert-butyl-2,4-dinitrobenzene → 4-(Tert-butyl)-3-nitroaniline

HRID 887502ノート

反応式

HRID 887502 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]([CH3:13])([CH3:12])[CH3:11])=[C:6]([N+:14]([O-:16])=[O:15])[CH:5]=1)([O-])=O.[S]>O>[C:10]([C:7]1[CH:8]=[CH:9][C:4]([NH2:1])=[CH:5][C:6]=1[N+:14]([O-:16])=[O:15])([CH3:13])([CH3:11])[CH3:12]

参加物

4

反応物 2

HCID 2385901-tert-butyl-2,4-dinitrobenzeneHCID 5362487Sulfur

生成物 1

HCID 3161634-(Tert-butyl)-3-nitroaniline

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A mixture of 1,3-dinitro-4-tert-butylbenzene (10.0 g) in H2O (56 ml) was heated to reflux. A mixture of Na2S (21.42 g) and sulfur (2.85 g) in H2O (34 ml) was added over 1 h via an addition funnel. The reaction maintained at reflux for 1.5 h then cooled to RT and extracted with EtOAc. The organic extracts were combined and washed with H2O, brine, dried over MgSO4 and concentrated in vacuo to afford 4-tert-butyl-3-nitro-phenylamine, which was used as is without further purification.

後処理

  1. temperaturewas heated to reflux
  2. additionwas added over 1 h via an addition funnel
  3. temperatureThe reaction maintained
  4. temperatureat reflux for 1.5 h
  5. extractionextracted with EtOAc
  6. washwashed with H2O, brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-eceedceb85ed4ba9b71b28b09066eef8
出典データセット
uspto-grants-2012_08
特許番号
US08247430B2

反応ノート

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