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Potassium Carbonate → HCID 14720290、化合物

HRID 2351973
ノート
印刷プレビュー

反応式

HRID 2351973 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH2:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:22]([S:24](Cl)(=[O:26])=[O:25])[CH3:23]>ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]([CH2:9][C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)[S:24]([CH2:22][CH3:23])(=[O:26])=[O:25])=[CH:6][CH:7]=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 3

HCID 11430Potassium CarbonateHCID 11667Ethanesulfonyl chlorideHCID 28045454-chloro-N-(pyridin-3-ylmethyl)aniline

生成物 1

HCID 14720290HCID 14720290、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A 4.37 g. portion of 3-(4-chlorophenylaminomethyl)pyridine was dissolved in 20 ml. of dichloromethane, and 4.1 g. of potassium carbonate and 3.8 g. of ethanesulfonyl chloride were added. The mixture was stirred under gentle reflux overnight, and was then allowed to stand for several days at ambient temperature. The mixture was extracted with water, dried over magnesium sulfate and filtered. The residue was taken up in chloroform and purified over silica gel, eluting with chloroform. The product-containing fractions were collected and evaporated under vacuum to obtain 1 g. of the desired product, m.p. 104°-106°.

後処理

  1. temperatureunder gentle reflux overnight
  2. waitto stand for several days at ambient temperature
  3. extractionThe mixture was extracted with water
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. custompurified over silica gel
  7. washeluting with chloroform
  8. customThe product-containing fractions were collected
  9. customevaporated under vacuum
  10. customto obtain 1 g

出典と根拠

ORDレコード
ord-178693faa9c04231adcd7564f9b54ffc
出典データセット
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04874775

反応ノート

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