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Methanesulfonamide → N-(Diphenoxymethylene)-methanesulfonamide

HRID 1892137
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반응식

HRID 1892137 반응식
Cl[C:2](Cl)([O:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH3:18][S:19]([NH2:22])(=[O:21])=[O:20]>CCOC(C)=O>[CH3:18][S:19]([N:22]=[C:2]([O:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[O:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)(=[O:21])=[O:20]
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참가 물질

4

반응물 2

HCID 72879MethanesulfonamideHCID 5116898Dichlorodiphenoxymethane

생성물 1

HCID 13738851N-(Diphenoxymethylene)-methanesulfonamide수율 35%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Dichlorodiphenoxymethane (2 g, 7.46 mmol) and methylsulfonamide (1.56 g, 16.41 mmol) were dissolved in EtOAc (15 ml) and heated to reflux for 12 hours. The mixture was allowed to cool and was concentrated under vacuum. Purification of the crude mixture by flash chromatography (20% EtOAc/hexanes) afforded diphenyl methylsulfonylcarbonimidate (0.75 g, 2.59 mmol, 35%).

후처리

  1. temperatureheated
  2. temperatureto reflux for 12 hours
  3. temperatureto cool
  4. concentrationwas concentrated under vacuum
  5. customPurification of the crude mixture by flash chromatography (20% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-ba0a139c0cc145c4b92af88b1ebbac74
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507672B2

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