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

HRID 256609

反応式

HRID 256609 の反応式
[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]

参加物

9

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 4

HCID 176Acetic Acid溶媒HCID 962Water溶媒HCID 1118Sulfuric Acid溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-446eddc3b81e48e8876107b742a089a5
出典データセット
uspto-grants-1993_11
特許番号
US05258399

関連ノート

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