Hydrochloric Acid → 2-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]acetic acid

HRID 654011

반응식

HRID 654011 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])=[CH:9][C:8]=1[C:14]([F:17])([F:16])[F:15].[OH-].[Na+].Cl.CCOCC.CCCCCC>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:19])=[O:18])=[C:8]([C:14]([F:17])([F:15])[F:16])[CH:9]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 150576042-[N-(4-Fluoro-2-trifluoromethylphenyl)sulfamoyl]-acetic acid methyl esterHCID 21584099Diethylether hexane

생성물 1

HCID 156765552-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]acetic acid

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

2.2 g (6.98 mmol) of 2-[N-(4-fluoro-2-trifluoromethylphenyl)sulfamoyl]-acetic acid methyl ester is dissolved in 20 ml of dioxane, and the solution is mixed with 10 ml (20 mmol) of 2N sodium hydroxide solution. A slight warming occurs and the saponification is complete after 10 minutes. The solution is neutralized with 2N hydrochloric acid with pH control and gently evaporated to dryness in a vacuum. The residue is extracted with 30 ml ethyl acetate, the solution is shaken out once with 10 ml of water, the organic phase is dried on magnesium sulfate, filtered and evaporated to dryness. 1.96 g (6.51 mmol)=93.2% of the theoretical yield is obtained. Melting point 120-121° C. (ether/hexane).

후처리

  1. temperatureA slight warming
  2. customgently evaporated to dryness in a vacuum
  3. extractionThe residue is extracted with 30 ml ethyl acetate
  4. customthe organic phase is dried on magnesium sulfate
  5. filtrationfiltered
  6. customevaporated to dryness
  7. custom1.96 g (6.51 mmol)=93.2% of the theoretical yield
  8. customis obtained

출처 및 근거

ORD 기록
ord-6d86645e0c254556a7447a41adb5575d
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05130119

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