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4-Fluorophenylhydrazine hydrochloride → N-[(E)-(3,5-dibromo-4-pyridinyl)methylideneamino]-4-fluoroaniline

HRID 1361117
ノート
印刷プレビュー

反応式

HRID 1361117 の反応式
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Br:10])[C:7]=1[CH:8]=O.Cl.[F:12][C:13]1[CH:18]=[CH:17][C:16]([NH:19][NH2:20])=[CH:15][CH:14]=1.C([O-])(=O)C.[Na+]>C(O)C.O>[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Br:10])[C:7]=1/[CH:8]=[N:20]/[NH:19][C:16]1[CH:17]=[CH:18][C:13]([F:12])=[CH:14][CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 699814-Fluorophenylhydrazine hydrochlorideHCID 517045Sodium AcetateHCID 27629983,5-Dibromo-4-pyridinecarboxaldehyde

生成物 1

HCID 59278325N-[(E)-(3,5-dibromo-4-pyridinyl)methylideneamino]-4-fluoroaniline

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of 3,5-dibromo-4-pyridinecarboxaldehyde (30.0 g, 113 mmol) in ethanol (1200 mL) at reflux was added 4-fluorophenylhydrazine hydrochloride (20.0 g, 123 mmol) in several portions followed by a solution of sodium acetate (31.0 g, 228 mmol) in water (200 mL). The mixture turned from a deep red to a bright yellow and over time a yellow solid precipitated. After 20 minutes, the mixture was cooled, diluted with water (1000 mL) and the yellow solid was collected by filtration. The solid was washed with water and dried to afford N-[1-(3,5-dibromopyridin-4-yl)-meth-(E)-ylidene]-N′-(4-fluorophenyl)-hydrazine.

後処理

  1. customprecipitated
  2. temperaturethe mixture was cooled
  3. additiondiluted with water (1000 mL)
  4. filtrationthe yellow solid was collected by filtration
  5. washThe solid was washed with water
  6. customdried

出典と根拠

ORDレコード
ord-2691df2535024c6698bdacb3f6f7a21f
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07879873B2

反応ノート

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