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Ethylenediamine → N1-(pyridin-4-yl)ethane-1,2-diamine

HRID 11450
ノート
印刷プレビュー

反応式

HRID 11450 の反応式
[CH2:1]([NH2:4])[CH2:2][NH2:3].Cl.Br[C:7]1[CH:12]=[CH:11][N:10]=[CH:9][CH:8]=1.C(=O)([O-])[O-].[K+].[K+]>>[N:10]1[CH:11]=[CH:12][C:7]([NH:3][CH2:2][CH2:1][NH2:4])=[CH:8][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 3301EthylenediamineHCID 11430Potassium CarbonateHCID 881004-Bromopyridinium chloride

生成物 1

HCID 14834209N1-(pyridin-4-yl)ethane-1,2-diamine収率 77%

実験手順

Ethylenediamine (10.4 ml, 155 mmol) was added to 4-bromopyridine hydrochloride (3.00 g, 15.5 mmol) under a nitrogen atmosphere, and the mixture was refluxed for 1.5 hours. The temperature was cooled to room temperature, potassium carbonate (8.57 g, 62.0 mmol) was added to the reaction mixture, and the whole was stirred for 10 minutes. Then, the solid was filtered out and washed with toluene and 2-propanol successively. The filtrate was concentrated under reduced pressure, the residue was purified by basic silica gel column chromatography, and the resulting solid was filtered off with diisopropyl ether to give 1.63 g (77%) of the titled compound as a pale yellow solid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturethe mixture was refluxed for 1.5 hours
  2. filtrationThen, the solid was filtered out
  3. washwashed with toluene and 2-propanol successively
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe residue was purified by basic silica gel column chromatography
  6. filtrationthe resulting solid was filtered off with diisopropyl ether

出典と根拠

ORDレコード
ord-058da2b8cb024016b60ad8909917c9ed
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07098226B2

反応ノート

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