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

HRID 277674
ノート
印刷プレビュー

反応式

HRID 277674 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

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

生成物 1

HCID 227093292-Difluoromethyloxy-4,6-dimethylphenyl acetic acid収率 14%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 6386tert-Butanol溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9f85cf0a0e9447d5ac7138907c46dfcd
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06358887B1

反応ノート

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