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Sulfuric Acid → 5-(2-fluorophenyl)-2,2-dimethyl-6-methyl-4H-1,3-dioxin-4-one

HRID 1648185
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1648185
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]([C:12]([CH3:14])=[O:13])[C:9]([OH:11])=[O:10].C(O[C:19](=O)[CH3:20])(=O)C.S(=O)(=O)(O)O.[C:27](=O)([O-])[O-].[Na+].[Na+]>CC(C)=O>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9](=[O:11])[O:10][C:19]([CH3:20])([CH3:27])[O:13][C:12]=1[CH3:14]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 1118Sulfuric AcidHCID 7918Acetic AnhydrideHCID 10340Sodium CarbonateHCID 3023024Acetyl(2-fluorophenyl)acetic acid

Produkt 1

HCID 153008465-(2-fluorophenyl)-2,2-dimethyl-6-methyl-4H-1,3-dioxin-4-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180
Acetone
Lösungsmittel

Versuchsvorschrift

A mixture of 2-(2-fluorophenyl)acetoacetic acid (5.1 g), acetone (4.2 ml), and acetic anhydride (5.4 ml) was kept at -20° C. and concentrated sulfuric acid (0.3 ml) was added thereto. This was kept at -15° C. and the reaction was carried out for 48 hours. The reaction mixture was added to an aqueous 10 % sodium carbonate solution (150 ml) which was ice-cooled, and the mixture was stirred for a short time at room temperature. White crystals which formed were collected by filtration, and washed well with water and then with hexane. The crystals obtained were dried well under reduced pressure to obtain the captioned compound (5.2 g).

Aufarbeitung

  1. customwas kept at -20° C.
  2. customThis was kept at -15° C.
  3. temperaturecooled
  4. customWhite crystals which formed
  5. filtrationwere collected by filtration
  6. washwashed well with water
  7. customThe crystals obtained
  8. customwere dried well under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-bdc3e776827c407685d5ec95f971d9c4
Quelldatensatz
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05436224

Notizen zur Reaktion

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