Methyl iodide → N-(2-acetylphenyl)-N-methylmethanesulfonamide

HRID 466356ノート

反応式

HRID 466356 の反応式
[C:1]([C:4]1[CH:14]=[CH:13][CH:12]=[CH:11][C:5]=1[NH:6][S:7]([CH3:10])(=[O:9])=[O:8])(=[O:3])[CH3:2].[H-].[Na+].CI.[C:19](OCC)(=O)C>O1CCCC1.CN(C)C=O>[O:3]=[C:1]([C:4]1[CH:14]=[CH:13][CH:12]=[CH:11][C:5]=1[N:6]([CH3:19])[S:7]([CH3:10])(=[O:8])=[O:9])[CH3:2]

参加物

7

反応物 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 2767200N-(2-acetylphenyl)methanesulfonamide

生成物 1

HCID 19873387N-(2-acetylphenyl)-N-methylmethanesulfonamide

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

2'-Acetylmethanesulfonanilide (1.0 g, 4.7 mmol) in 10 ml tetrahydrofuran is reacted with 0.23 g (4.8 mmol) of 50% sodium hydride dispersion in mineral oil at 5° C. for 15 min. Methyl iodide (1.5 g, 10.56 mmol) in 10 ml of dimethylformamide is added over 15 min at 0°-10° C. and stirred in cold for 15 min. Dimethylformamide (10 ml) is added, and the reaction is stirred for 2 days at room temperature. The reaction is taken up into ethyl acetate, the organic layer washed with water, sodium carbonate solution, water, and saturated sodium chloride successively. The dried organic layer is evaporated and the product crystallized from ether-pet. ether; m.p. 98°-99° C.

後処理

  1. stirringthe reaction is stirred for 2 days at room temperature
  2. washthe organic layer washed with water, sodium carbonate solution, water, and saturated sodium chloride successively
  3. customThe dried organic layer is evaporated
  4. customthe product crystallized from ether-pet. ether

出典と根拠

ORDレコード
ord-1b06c96958d546a188a3816ad364e196
出典データセット
uspto-grants-1992_10
特許番号
US05155268

反応ノート

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