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Potassium Carbonate → HCID 14720310, 화합물

HRID 2351982
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HRID 2351982 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:22][S:23](Cl)(=[O:25])=[O:24]>ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]([CH2:9][C:10]2[CH:11]=[CH:12][N:13]=[CH:14][CH:15]=2)[S:23]([CH3:22])(=[O:25])=[O:24])=[CH:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chloride2회HCID 9643524-chloro-N-(pyridin-4-ylmethyl)aniline

생성물 1

HCID 14720310HCID 14720310, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A 3.3 g. portion of 4-(4-chlorophenylaminomethyl)pyridine was dissolved in 15 ml. of dichloromethane, and 2.7 g. of potassium carbonate and 1.6 ml. of methanesulfonyl chloride were added. The mixture was stirred at ambient temperature for several days, adding another 0.5 ml. of methanesulfonyl chloride in the process. The mixture was then diluted with dichloromethane, extracted with aqueous sodium bicarbonate and with water, dried over magnesium sulfate and evaporated. The residue was taken up in dichloromethane and chromatographed over silica gel, eluting first with dichloromethane and then with 9:1 dichloromethane:ethyl acetate. The product-containing fractions were combined and evaporated, and the residue was triturated with petroleum ether and diethyl ether to obtain 2.1 g. of the desired product.

후처리

  1. additionadding another 0.5 ml
  2. extractionextracted with aqueous sodium bicarbonate and with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated
  5. customchromatographed over silica gel
  6. washeluting first with dichloromethane
  7. customevaporated
  8. customthe residue was triturated with petroleum ether and diethyl ether
  9. customto obtain 2.1 g

출처 및 근거

ORD 기록
ord-420ce333902c4b84bd59d6da2ed2a76f
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04874775

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