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

HRID 1488491노트

반응식

HRID 1488491 반응식
[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

참가 물질

5

반응물 2

HCID 9951467HCID 9951467, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-369e5e5fe0504009adede4b3e3cae243
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05674886

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