Sulfuric Acid → 3,4-Difluoro-benzenesulfinic acid

HRID 1820796노트

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HRID 1820796 반응식
S([O-])([O-])=O.[Na+].[Na+].[F:7][C:8]1[CH:9]=[C:10]([S:15](Cl)(=[O:17])=[O:16])[CH:11]=[CH:12][C:13]=1[F:14].[OH-].[Na+].OS(O)(=O)=O>O.O1CCOCC1>[F:7][C:8]1[CH:9]=[C:10]([S:15]([OH:17])=[O:16])[CH:11]=[CH:12][C:13]=1[F:14]

참가 물질

7

반응물 4

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 24437Sodium SulfiteHCID 27369133,4-Difluorobenzene-1-sulfonyl chloride

생성물 1

HCID 138368283,4-Difluoro-benzenesulfinic acid

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

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온도
0 °C

실험 절차

To 2.47 mol sodium sulfite in 1120 ml water at RT was added dropwise over 20 min a solution of 329 mmol 3,4-difluoro-benzenesulfonyl chloride in 560 ml dioxane and stirring continued for a further 30 min. 1 M aq NaOH was then added dropwise until the reaction mixture was pH 14, and the mixture was then allowed to stir at RT for a further 16 h. The mixture was then cooled to 0° C. and concentrated H2SO4 added until the reaction mixture was pH 1. The mixture was extracted three times with ethyl acetate, and the combined organic phases washed with saturated aq NaCl solution and then dried with Na2SO4. Evaporation in vacuo yielded the title compound. MS (m/e): 177.1 ([M−H]−, 100%)

후처리

  1. stirringto stir at RT for a further 16 h
  2. extractionThe mixture was extracted three times with ethyl acetate
  3. washthe combined organic phases washed with saturated aq NaCl solution
  4. dry with materialdried with Na2SO4
  5. customEvaporation in vacuo

출처 및 근거

ORD 기록
ord-b1dc1647ca094fa1a9a52d5227b5db88
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07605163B2

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