Sodium Hydroxide → 2-[N-(4-fluoro-3-trifluoromethylphenyl)sulfamoyl]acetic acid

HRID 248754노트

반응식

HRID 248754 반응식
C[O:2][C:3](=[O:20])[CH2:4][S:5](=[O:19])(=[O:18])[NH:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([C:14]([F:17])([F:16])[F:15])[CH:8]=1.[OH-].[Na+]>O1CCOCC1>[F:13][C:10]1[CH:11]=[CH:12][C:7]([NH:6][S:5]([CH2:4][C:3]([OH:20])=[O:2])(=[O:18])=[O:19])=[CH:8][C:9]=1[C:14]([F:17])([F:15])[F:16]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 542944922-[N-(4-Fluoro-3-trifluoromethylphenyl)sulfamoyl]acetic Acid Methyl Ester

생성물 1

HCID 197640082-[N-(4-fluoro-3-trifluoromethylphenyl)sulfamoyl]acetic acid

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

12.79 g (40.57 mmol) of 2-[N-(4-fluoro-3-trifluoromethylphenyl)sulfamoyl]acetic acid methyl ester is dissolved in 110 ml of dioxane and combined with 59 ml (118 mmol) of 2N sodium hydroxide solution. The mixture heated up slightly, and the starting material had disappeared after 15 minutes. The mixture is concentrated to dryness under vacuum, the residue is combined with 2N hydrochloric acid, and the thus-precipitated acid is taken up in ethyl acetate. The organic solution is washed with water, dried over sodium sulfate, and concentrated to dryness under vacuum. The residue is crystallized from ethyl acetate/hexane. The title compound melts at 138°-140° C.

후처리

  1. temperatureThe mixture heated up slightly
  2. concentrationThe mixture is concentrated to dryness under vacuum
  3. washThe organic solution is washed with water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to dryness under vacuum
  6. customThe residue is crystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-6ec1e4c8022044ff814b8fc0514a91dc
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05210290

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