Benzyl-(2-chloro-3-nitro-6-trifluoromethyl-pyridin-4-yl)-amine → N4-Benzyl-2-chloro-6-trifluoromethyl-pyridine-3,4-diamine

HRID 639619ノート

反応式

HRID 639619 の反応式
[CH2:1]([NH:8][C:9]1[CH:14]=[C:13]([C:15]([F:18])([F:17])[F:16])[N:12]=[C:11]([Cl:19])[C:10]=1[N+:20]([O-])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CC(O)=O.O.[Fe]>[CH2:1]([NH:8][C:9]1[CH:14]=[C:13]([C:15]([F:18])([F:16])[F:17])[N:12]=[C:11]([Cl:19])[C:10]=1[NH2:20])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 1

HCID 86614472Benzyl-(2-chloro-3-nitro-6-trifluoromethyl-pyridin-4-yl)-amine

生成物 1

HCID 86614471N4-Benzyl-2-chloro-6-trifluoromethyl-pyridine-3,4-diamine収率 100,764.102%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

Benzyl-(2-chloro-3-nitro-6-trifluoromethyl-pyridine-4-yl)-amine (345 mg, 1.0 mmol) was dissolved in a mixture of AcOH (18 ml) and water (2 ml). Fe powder (349 mg, 6.2 mmol) was added and the mixture was vigorously stirred at room temperature for 24 h. The reaction mixture was concentrated in vacuo and the residue was diluted with EtOAc (10 ml) and water (10 ml). The mixture was filtered through celite, washing through with EtOAc (20 ml). The layers were separated and the organic layer was washed with sat. NaHCO3 (aq) (2×10 ml) and brine (10 ml), dried over MgSO4 and concentrated in vacuo to give the title compound (304 g) as a pale yellow solid.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionthe residue was diluted with EtOAc (10 ml) and water (10 ml)
  3. filtrationThe mixture was filtered through celite
  4. washwashing through with EtOAc (20 ml)
  5. customThe layers were separated
  6. washthe organic layer was washed with sat. NaHCO3 (aq) (2×10 ml) and brine (10 ml)
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-a7fde78db8554c5db0557ec9b6f396e9
出典データセット
uspto-grants-2010_04
特許番号
US07691877B2

反応ノート

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