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Potassium Carbonate → HCID 14720290, 화합물

HRID 2351973
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HRID 2351973 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 14720290HCID 14720290, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-178693faa9c04231adcd7564f9b54ffc
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04874775

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