Sodium Hydroxide → N-[3-(dimethylamino)phenyl]methanesulphonamide

HRID 244524

반응식

HRID 244524 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][N:7]([CH3:15])[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([NH2:14])[CH:9]=1.[OH-].[Na+]>O>[CH3:6][N:7]([CH3:15])[C:8]1[CH:9]=[C:10]([NH:14][S:2]([CH3:1])(=[O:4])=[O:3])[CH:11]=[CH:12][CH:13]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 31297Methanesulfonyl chlorideHCID 76084N,N-dimethyl-m-phenylenediamine

생성물 1

HCID 13796402N-[3-(dimethylamino)phenyl]methanesulphonamide수율 79%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Methanesulphonyl chloride (838 mg, 7.35 mmol) was added slowly to a cooled solution (5° C.) of N,N-dimethyl-1,3-phenylenediamine (1.00 g, 7.35 mmol) and sodium hydroxide (5M, 1.5 cm3) in water (10 cm3). The reaction was allowed to warm to room temperature overnight. The mixture was extracted with chloroform (3×15 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. Column chromatography (1:20 methanol/dichloromethane) gave the target material as a brown oil (1.24 g, 79%).

후처리

  1. extractionThe mixture was extracted with chloroform (3×15 cm3)
  2. dry with materialThe combined extracts were dried over sodium sulphate
  3. filtrationfiltered
  4. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-b8fd1201b5654d798122c4747976812a
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658665B2

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