Potassium Carbonate → HCID 14720303, 화합물

HRID 2351977노트

반응식

HRID 2351977 반응식
ClC.[CH3:3][C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[CH:6][C:5]=1[NH:11][CH2:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:25]([S:29](Cl)(=[O:31])=[O:30])[CH2:26][CH2:27][CH3:28]>C(=O)(O)[O-].[Na+]>[CH3:3][C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[CH:6][C:5]=1[N:11]([CH2:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=1)[S:29]([CH2:25][CH2:26][CH2:27][CH3:28])(=[O:31])=[O:30]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 754301-Butanesulfonyl chlorideHCID 19844836HCID 19844836, 화합물

생성물 1

HCID 14720303HCID 14720303, 화합물

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

실험 절차

A 4.2 g. portion of 3-(2,4-dimethylphenylaminomethyl)pyridine chloromethane, and to it were added 4.1 g. of potassium carbonate and 4.7 g. of butanesulfonyl chloride. The mixture was stirred at ambient temperature for 4 days, and then was stirred under gentle reflux for several days more. It was then diluted with aqueous sodium bicarbonate and extracted with dichloromethane, and the organic layer was dried over magnesium sulfate and evaporated to an oil. The oil was applied to a silica gel column and eluted with dichloromethane and then with chloroform to obtain 0.75 g. of the desired product.

후처리

  1. stirringwas stirred
  2. temperatureunder gentle reflux for several days more
  3. extractionextracted with dichloromethane
  4. dry with materialthe organic layer was dried over magnesium sulfate
  5. customevaporated to an oil
  6. washeluted with dichloromethane
  7. customwith chloroform to obtain 0.75 g

출처 및 근거

ORD 기록
ord-f1232f9bdfa44a5f9760ea108619adba
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04874775

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