Trifluoroacetic acid → 2-(2-Fluoroethylthio)-phenylsulfonamide

HRID 1534174노트

반응식

HRID 1534174 반응식
FC(F)(F)C(O)=O.[F:8][CH2:9][CH2:10][S:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[S:18]([NH:21]C(C)(C)C)(=[O:20])=[O:19]>ClC(Cl)Cl>[F:8][CH2:9][CH2:10][S:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[S:18]([NH2:21])(=[O:19])=[O:20]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 199109362-(2-fluoroethylthio)-N-tert.-butylphenylsulfonamide

생성물 1

HCID 198097542-(2-Fluoroethylthio)-phenylsulfonamide

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

25 ml of trifluoroacetic acid are added at a temperature of 0° C. to a solution of 3.88 g of 2-(2-fluoroethylthio)-N-tert.-butylphenylsulfonamide, obtained in accordance with Example P1, in 25 ml of trichloromethane. After stirring for 18 hours at a temperature of +25° C., the resulting brown reaction mixture is lyophilised. After chromatographic purification of the oily residue with 1) ethyl acetate/petroleum ether (1:1) over silica gel and 2) dichloromethane/acetone (9:1) over silica gel, the resulting fractions are concentrated by evaporation to give 1.5 g (60.5% of the theoretical yield) of crystalline 2-(2-fluoroethylthio)-phenylsulfonamide.

후처리

  1. customAfter chromatographic purification of the oily residue with 1) ethyl acetate/petroleum ether (1:1) over silica gel and 2) dichloromethane/acetone (9:1) over silica gel
  2. concentrationthe resulting fractions are concentrated by evaporation
  3. customto give 1.5 g (60.5% of the

출처 및 근거

ORD 기록
ord-8c7a26a5f0f042409d8bf6feb52d9d17
출처 데이터셋
uspto-grants-1992_02
특허 번호
US05087749

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