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Potassium Carbonate → HCID 14720293, 화합물

HRID 2351974
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HRID 2351974 반응식
[CH:1]1([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([NH:15][CH2:16][C:17]3[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=3)=[CH:11][CH:10]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].[CH3:29][S:30](Cl)(=[O:32])=[O:31]>ClCCl>[CH:1]1([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([N:15]([CH2:16][C:17]3[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=3)[S:30]([CH3:29])(=[O:32])=[O:31])=[CH:11][CH:10]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 14720292HCID 14720292, 화합물

생성물 1

HCID 14720293HCID 14720293, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A 3.5 g. portion of 3-(4-cyclohexylmethoxyphenylaminomethyl)pyridine was dissolved in 15 ml. of dichloromethane, and 2.76 g. of potassium carbonate and 1.55 ml. of methanesulfonyl chloride were added. The mixture was stirred with gentle heating for 20 hours, and was then extracted with aqueous sodium bicarbonate, dried over magnesium sulfate and evaporated under vacuum. The residue was dissolved in chloroform and chromatographed over silica gel, eluting with chloroform. The product-containing fractions were combined and evaporated, and the residue was triturated with diethyl ether, filtered and dried to obtain 2.33 g. of impure product, which was further washed with diethyl ether to obtain 1.88 g. of the desired product, m.p. 36°-140°.

후처리

  1. temperaturewith gentle heating for 20 hours
  2. extractionwas then extracted with aqueous sodium bicarbonate
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under vacuum
  5. dissolutionThe residue was dissolved in chloroform
  6. customchromatographed over silica gel
  7. washeluting with chloroform
  8. customevaporated
  9. customthe residue was triturated with diethyl ether
  10. filtrationfiltered
  11. customdried
  12. customto obtain 2.33 g
  13. washof impure product, which was further washed with diethyl ether
  14. customto obtain 1.88 g

출처 및 근거

ORD 기록
ord-3b28eb96dfde4049bd3074c1d559ab49
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04874775

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