HCID 9951467、化合物 → 4-[N-(4-aminophenyl)-N-(4-bromobenzyl)amino]-4H-1,2,4-triazole

HRID 1488491ノート

反応式

HRID 1488491 の反応式
[Br:1][C:2]1[CH:23]=[CH:22][C:5]([CH2:6][N:7]([N:17]2[CH:21]=[N:20][N:19]=[CH:18]2)[C:8]2[CH:13]=[CH:12][C:11]([N+:14]([O-])=O)=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[H][H]>[Ni].C(O)C>[NH2:14][C:11]1[CH:12]=[CH:13][C:8]([N:7]([N:17]2[CH:18]=[N:19][N:20]=[CH:21]2)[CH2:6][C:5]2[CH:4]=[CH:3][C:2]([Br:1])=[CH:23][CH:22]=2)=[CH:9][CH:10]=1

参加物

5

反応物 2

HCID 9951467HCID 9951467、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 229058094-[N-(4-aminophenyl)-N-(4-bromobenzyl)amino]-4H-1,2,4-triazole収率 32%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒

実験手順

A catalytic amount of Raney nickel was added to 50 ml of an ethanol solution containing 3.74 g of 4-[N-(4-bromobenzyl)-N-(4-nitrophenyl) amino]-4H-1,2,4-triazole, and the mixture was stirred for about 2 hours in the presence of hydrogen gas at room temperature. After the catalyst was removed by filtration, the resulting filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography to give 1.1 g of 4-[N-(4-aminophenyl)-N-(4-bromobenzyl)amino]-4H-1,2,4-triazole from the chloroform/methanol (50:1) eluate.

後処理

  1. customAfter the catalyst was removed by filtration
  2. concentrationthe resulting filtrate was concentrated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-369e5e5fe0504009adede4b3e3cae243
出典データセット
uspto-grants-1997_10
特許番号
US05674886

反応ノート

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