Methylamine → N-Methyl-4-nitrobenzenesulfonamide

HRID 29047노트

반응식

HRID 29047 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10](Cl)(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH3:14][NH2:15]>CCOCC>[CH3:14][NH:15][S:10]([C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)(=[O:12])=[O:11]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 74044-Nitrobenzenesulfonyl chloride

생성물 1

HCID 232993N-Methyl-4-nitrobenzenesulfonamide수율 98.4%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a suspension of 4-nitrobenzenesulfonyl chloride (5 g, 22.56 mmol) in ether (250 ml), methylamine (5 ml, 40% aq. solution, 56.4 mmol) was added, and the mixture was stirred at room temperature. After 16 hr. the reaction mixture was concentrated to remove the solvent and the residue was resuspended in methylene chloride. After washing with 2N HCl and brine, the organic fractions were dried (MgSO4), filtered and concentrated to give N-methyl-4-nitrobenzenesulfonamide (4.8 g, 98%): mp (DSC) 109° C. Anal Calc'd. for C7H8N2O4S: C, 38.89; H, 3.73; N, 12.96. Found: C, 38.83; H, 3.72; N, 12.96.

후처리

  1. additionwas added
  2. concentrationthe reaction mixture was concentrated
  3. customto remove the solvent
  4. washAfter washing with 2N HCl and brine
  5. dry with materialthe organic fractions were dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ccb6d66ead81471897de02c5abc5b139
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07420061B2

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