Iodine → N-(4-iodo-3-methylphenyl)-N-methylmethanesulphonamide

HRID 256609

반응식

HRID 256609 반응식
[CH3:1][N:2]([C:7]1[CH:8]=[C:9]([CH3:13])[CH:10]=[CH:11][CH:12]=1)[S:3]([CH3:6])(=[O:5])=[O:4].II.[I:16](O)(=O)=O.C(=O)(O)[O-].[Na+]>C(O)(=O)C.S(=O)(=O)(O)O.O.C(OCC)(=O)C>[I:16][C:10]1[CH:11]=[CH:12][C:7]([N:2]([CH3:1])[S:3]([CH3:6])(=[O:4])=[O:5])=[CH:8][C:9]=1[CH3:13]

참가 물질

9

반응물 4

HCID 807IodineHCID 24345Iodic acidHCID 516892Sodium BicarbonateHCID 19785598N-Methyl-N-(3-tolyl)methanesulphonamide

생성물 1

HCID 19785617N-(4-iodo-3-methylphenyl)-N-methylmethanesulphonamide수율 340%

시약·촉매·용매 4

HCID 176Acetic Acid용매HCID 962Water용매HCID 1118Sulfuric Acid용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of N-methyl-N-(3-tolyl)methanesulphonamide (0.12 g), iodine (76 g) and iodic acid (35 mg) in glacial acetic acid (5 ml) and concentrated sulphuric acid (0.6 ml) was stirred at 80° C. for 2.5 hours. Ethyl acetate (40 ml) and water (40 ml) were then added and the mixture neutralised with solid sodium bicarbonate. The organic phase was washed with brine (30 ml), dried (MgSO4) and the solvent evaporated to leave N-(4-iodo-3-methylphenyl)-N-methylmethanesulphonamide (0.22 g, 90%), m.p. 85°-87° C.

후처리

  1. washThe organic phase was washed with brine (30 ml)
  2. dry with materialdried (MgSO4)
  3. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-446eddc3b81e48e8876107b742a089a5
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258399

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