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Pyridine → N1-(6-Chloropyridin-2-yl)-N2,N2-dimethylethane-1,2-diamine

HRID 1395530
ノート
印刷プレビュー

反応式

HRID 1395530 の反応式
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[N:3]=1.C[NH:10][CH2:11][CH2:12][NH:13][CH3:14].N1C=CC=C[CH:16]=1>>[CH3:16][N:13]([CH3:14])[CH2:12][CH2:11][NH:10][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[N:3]=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 1049PyridineHCID 8070N,N'-DimethylethylenediamineHCID 169892,6-Dichloropyridine

生成物 1

HCID 20339561N1-(6-Chloropyridin-2-yl)-N2,N2-dimethylethane-1,2-diamine収率 70%

実験手順

A solution of 2,6-dichloropyridine (29.6 g., 0.20 mole) and unsymmetrical dimethylethylenediamine (52.9 g., 0.60 mole) in 100 ml of pyridine is stirred at reflux for 48 hours. The pyridine is removed under reduced pressure and the residual mixture is poured into water and made basic with excess sodium hydroxide. The product is extracted into ethyl acetate which is then concentrated and the residual oil is distilled. 2-(2-Dimethylaminoethylamino)-6-chloropyridine boiling at 104°-105° at 0.2 mm is collected in 70% yield.

後処理

  1. temperatureat reflux for 48 hours
  2. customThe pyridine is removed under reduced pressure
  3. additionthe residual mixture is poured into water
  4. extractionThe product is extracted into ethyl acetate which
  5. concentrationis then concentrated
  6. distillationthe residual oil is distilled
  7. custom2-(2-Dimethylaminoethylamino)-6-chloropyridine boiling at 104°-105° at 0.2 mm is collected in 70% yield

出典と根拠

ORDレコード
ord-3aad83be6d564b87924b3fa512e8ba83
出典データセット
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04203988

反応ノート

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