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2-Methyl-2-butene → 2-Difluoromethyloxy-4,6-dimethylphenyl acetic acid

HRID 352352
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HRID 352352 반응식
[F:1][CH:2]([F:15])[O:3][C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([CH3:11])[C:5]=1[CH2:12][CH:13]=[O:14].CC(=CC)C.P([O-])(O)(O)=[O:22].[Na+].Cl([O-])=O.[Na+]>C(O)(C)(C)C.O.C(OCC)(=O)C>[F:1][CH:2]([F:15])[O:3][C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([CH3:11])[C:5]=1[CH2:12][C:13]([OH:22])=[O:14]
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참가 물질

8

반응물 4

HCID 105532-Methyl-2-buteneHCID 186846932-Difluoromethyloxy-4,6-dimethylphenylacetaldehydeHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphate

생성물 1

HCID 227093292-Difluoromethyloxy-4,6-dimethylphenyl acetic acid수율 14%

시약·촉매·용매 3

HCID 962
Water
용매
HCID 6386tert-Butanol용매
HCID 8857Ethyl Acetate용매

실험 절차

19.2 g of 2-difluoromethyloxy-4,6-dimethylphenylacetaldehyde (XXXIV-c-1) as the crude product were dissolved in 270 ml of tert-butanol, the solution was mixed with 90.4 g of 2-methyl-2-butene, and a solution of 90 g of sodium dihydrogen phosphate and 42 g of sodium chlorite in 353 ml of water was subsequently added dropwise at room temperature. The mixture was stirred for four hours and then stirred into 400 ml of ethyl acetate, and the phases were separated. The aqueous phase was extracted two more times using ethyl acetate, and the combined organic phases were dried over magnesium sulphate and concentrated. After stirring with hexane, 11 g of solid were isolated, from which 2.5 g (14% of theory via 2 steps) of 2-difluoromethyloxy-4,6-dimethylphenylacetic acid of melting point 124-127° C. were obtained.

후처리

  1. customthe phases were separated
  2. extractionThe aqueous phase was extracted two more times
  3. dry with materialthe combined organic phases were dried over magnesium sulphate
  4. concentrationconcentrated
  5. stirringAfter stirring with hexane

출처 및 근거

ORD 기록
ord-791c1f8aa2a6468f94d242303c753131
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06746990B2

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