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Hydrochloric Acid → 3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carboxylic acid

HRID 242297
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HRID 242297 반응식
[Na].[F:2][CH:3]([F:14])[C:4]1[C:8]([C:9](F)=[O:10])=[C:7]([F:12])[N:6]([CH3:13])[N:5]=1.Cl.S1(=O)(=[O:21])CCCC1>>[F:12][C:7]1[N:6]([CH3:13])[N:5]=[C:4]([CH:3]([F:14])[F:2])[C:8]=1[C:9]([OH:21])=[O:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 31347SulfolaneHCID 5360545SodiumHCID 585266223-(Difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carbonyl fluoride

생성물 1

HCID 231925843-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carboxylic acid

실험 절차

To 400 ml of a 1N sodium hydroxyde aqueous solution, was added dropwise 67.5 g of a solution (10% molar) of 3-(difluoromethyl)-5-fluoro-1-methyl-1H-pyrazole-4-carbonyl fluoride in tetrahydrothiophene 1,1-dioxide. The temperature was kept below 20° C. during the addition. After 2 hours of stirring at room temperature, the reaction mixture was carefully acidified to pH 2 with concentrated aqueous hydrochloric acid. The resulting white precipitate was filtered, washed with water, and dried to yield 6 g of 5-fluoro-3-(difluoromethyl)-1-methyl-1H-pyrazole-4-carboxylic acid as a white solid.

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후처리

  1. additionThe temperature was kept below 20° C. during the addition
  2. filtrationThe resulting white precipitate was filtered
  3. washwashed with water
  4. customdried

출처 및 근거

ORD 기록
ord-8f88cdcb5ac5475da72ffec2861f6483
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08653114B2

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