3-Nitro[1,1'-biphenyl]-2-amine → 102877-92-9

HRID 887991ノート

反応式

HRID 887991 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][CH:5]=[CH:4][C:3]=1[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>[Fe].CC(O)=O>[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

参加物

4

反応条件

温度
60 °C

実験手順

2-Amino-3-nitrobiphenyl d (0.613 g, 2.86 mmol) was purged under nitrogen for 30 minutes then HOAc (5 mL) was added followed by iron powder (0.4895 g, 8.76 mmol). The sample was heated at 60° C. for 30 minutes then HOAc (5 mL) was added. The sample was stirred at 60° C. for 1 hour then poured into ice. The sample was extracted with EtOAc (3×100 mL). The EtOAc extracts were washed with saturated NaHCO3 (3×100 mL. The EtOAc layer was dried over MgSO4, filtered, and concentrated to give 2,3-diaminobiphenyl e (0.439 g, 2.38 mmol, 83%).

後処理

  1. customwas purged under nitrogen for 30 minutes
  2. additionHOAc (5 mL) was added
  3. additionthen poured into ice
  4. extractionThe sample was extracted with EtOAc (3×100 mL)
  5. washThe EtOAc extracts were washed with saturated NaHCO3 (3×100 mL
  6. dry with materialThe EtOAc layer was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-3e1596c03f7c497e84cde641c0879ba6
出典データセット
uspto-grants-2012_08
特許番号
US08247557B2

反応ノート

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