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Benzylamine → benzyl(5-bromo-4-nitro-2-propyl-2H-pyrazol-3-yl)amine

HRID 1181154
ノート
印刷プレビュー

反応式

HRID 1181154 の反応式
[CH2:1]([N:4]1[C:8]([Br:9])=[C:7]([N+:10]([O-:12])=[O:11])[C:6]([Br:13])=[N:5]1)[CH2:2][CH3:3].[CH2:14]([NH2:21])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>CCO>[CH2:14]([NH:21][C:8]1[N:4]([CH2:1][CH2:2][CH3:3])[N:5]=[C:6]([Br:13])[C:7]=1[N+:10]([O-:12])=[O:11])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.[Br:9][C:8]1[C:7]([N+:10]([O-:12])=[O:11])=[C:6]([Br:13])[NH:5][N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 7504BenzylamineHCID 130072253,5-dibromo-1-propyl-4-nitro-1H-pyrazole

生成物 2

HCID 13007229benzyl(5-bromo-4-nitro-2-propyl-2H-pyrazol-3-yl)amineHCID 137079943,5-Dibromo-4-nitro-1H-pyrazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 1-propyl-3,5-dibromo-4-nitropyrazole (19.4 g, 62 mmol), EtOH (500 ml) and benzylamine (40 g, 373 mmol) was refluxed for 15 hours. The reaction medium was concentrated to the maximum under reduced pressure. The residue was suspended in EtOAc (100 ml ), the insoluble part was separated out by filtration and the filtrate was evaporated to dryness. The black oil obtained was purified by column chromatography (eluent: EtOAc/hexane) to give the benzyl(5-bromo-4-nitro-2-propyl-2H-pyrazol-3-yl)amine in the form of a yellow solid (9 g; 29%) from 3,5-dibromo-4-nitropyrazole.

後処理

  1. temperaturewas refluxed for 15 hours
  2. concentrationThe reaction medium was concentrated to the maximum under reduced pressure
  3. customthe insoluble part was separated out by filtration
  4. customthe filtrate was evaporated to dryness
  5. customThe black oil obtained
  6. customwas purified by column chromatography (eluent: EtOAc/hexane)

出典と根拠

ORDレコード
ord-6a276ecd548e4b60acf3d70fd8f60de2
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07285136B2

反応ノート

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