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

HRID 466356노트

반응식

HRID 466356 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1b06c96958d546a188a3816ad364e196
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155268

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