Triethylamine → N-methyl-1-(p-tolyl)methanesulfonamide

HRID 2254662

반응식

HRID 2254662 반응식
[CH3:1][C:2]1[CH:9]=[CH:8][C:5](NC)=[CH:4][CH:3]=1.C([N:12]([CH2:15]C)CC)C.[CH3:17][S:18](Cl)(=[O:20])=[O:19]>ClCCl>[CH3:15][NH:12][S:18]([CH2:17][C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:9][CH:8]=1)(=[O:20])=[O:19]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12165Benzenamine, N,4-dimethyl-HCID 31297Methanesulfonyl chloride

생성물 1

HCID 19917625N-methyl-1-(p-tolyl)methanesulfonamide수율 65%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of p-methyl-N-methylaniline (5.00 g) and triethylamine (5.05 g) in dichloromethane (140 ml) was cooled to 0° C. and methanesulphonyl chloride (4.73 g) was added dropwise. The reaction mixture was stirred at ambient temperature for 2 hours and quenched with water (100 ml). The organic phase was washed with 2N aqueous hydrochloric acid solution (75 ml) and 2N aqueous sodium hydroxide solution (75 ml), dried (MgSO4) and the solvent removed by evaporation. Thus was obtained N-methyl-(4-tolyl)methanesulphonamide (5.3 g, 65%), m.p. 49°-52° C.

후처리

  1. customquenched with water (100 ml)
  2. washThe organic phase was washed with 2N aqueous hydrochloric acid solution (75 ml) and 2N aqueous sodium hydroxide solution (75 ml)
  3. dry with materialdried (MgSO4)
  4. customthe solvent removed by evaporation

출처 및 근거

ORD 기록
ord-0d7d6b961b69478d9aa3095cb229d36a
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05236948

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