N-Acetylsulfanilyl chloride → N-[4-(2-dimethylaminoethylsulfamoyl)phenyl]acetamide

HRID 2185175노트

반응식

HRID 2185175 반응식
[C:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([S:11](Cl)(=[O:13])=[O:12])=[CH:7][CH:6]=1)(=[O:3])[CH3:2].[CH3:15][N:16]([CH3:20])[CH2:17][CH2:18][NH2:19]>ClCCl>[CH3:15][N:16]([CH3:20])[CH2:17][CH2:18][NH:19][S:11]([C:8]1[CH:9]=[CH:10][C:5]([NH:4][C:1](=[O:3])[CH3:2])=[CH:6][CH:7]=1)(=[O:13])=[O:12]

참가 물질

4

반응물 2

HCID 8481N-Acetylsulfanilyl chlorideHCID 66053N,N-Dimethylethylenediamine

생성물 1

HCID 3462536N-[4-(2-dimethylaminoethylsulfamoyl)phenyl]acetamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-Acetylaminobenzenesulfonyl chloride is introduced into dichloromethane and treated at room temperature with two equivalents of N,N-dimethylethylenediamine and stirred at room temperature until complete conversion can be determined (LCMS). For work-up, the solvent is distilled off, the oily residue is taken up in dichloromethane or ethyl acetate and the mixture is washed with NaHCO3 solution. The phases are separated and the aqueous phase is extracted once more with dichloromethane or ethyl acetate. The organic phases are dried using Na2SO4 and concentrated. The crude product thus obtained is reacted further without further purification. (MS-CI+: 286.0; LCMS Rt=2.542 min)

후처리

  1. distillationFor work-up, the solvent is distilled off
  2. washethyl acetate and the mixture is washed with NaHCO3 solution
  3. customThe phases are separated
  4. extractionthe aqueous phase is extracted once more with dichloromethane or ethyl acetate
  5. customThe organic phases are dried
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-070247a3a76b4c02843ef4a41d25cada
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06399824B1

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