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Acetic acid, 2-chloro-2-fluoro-, ethyl ester → HCID 54260202, Verbindung

HRID 1382149
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1382149
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[N:10]1[C:14](=[O:15])[N:13]([CH:16]([F:18])[F:17])[C:12]([CH3:19])=[N:11]1.Cl[CH:21]([F:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23].[Na]>C(O)C.C(OCC)C>[Cl:8][C:6]1[CH:7]=[C:2]([Cl:1])[C:3]([N:10]2[C:14](=[O:15])[N:13]([CH:16]([F:17])[F:18])[C:12]([CH3:19])=[N:11]2)=[CH:4][C:5]=1[O:9][CH:21]([F:27])[C:22]([O:24][CH2:25][CH3:26])=[O:23]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 101668Acetic acid, 2-chloro-2-fluoro-, ethyl esterHCID 5360545SodiumHCID 13253747HCID 13253747, Verbindung

Produkt 1

HCID 54260202HCID 54260202, VerbindungAusbeute 35,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittel2×
HCID 3283
Diethyl Ether
Lösungsmittel

Versuchsvorschrift

To a stirred mixture of 2.0 g (0.0065 mole) of 1-(2,4-dichloro-5-hydroxyphenyl)-4-difluoromethyl-4,5-dihydro-3-methyl-1,2,4-triazol-5(1H)-one and 0.91 g (0.0065 mole) of ethyl chlorofluoroacetate in 50 mL of ethanol was added a solution of 0.15 g (0.0065 mole) of sodium in 5 mL of ethanol. The reaction mixture was heated at reflux for 34 hours. The mixture was cooled, and the solvent was removed by evaporation under reduced pressure, leaving a residue. This residue was dissolved in diethyl ether, and the solution was washed first with water, followed by an aqueous 10% sodium hydroxide solution. The organic phase was dried over anhydrous magnesium sulfate, then filtered. The filtrate was evaporated under reduced pressure to yield 0.95 g of ethyl [2,4-dichloro-5-(4-difluoromethyl-4,5-dihydro-3-methyl-5-oxo-1H-1,2,4-triazol-1-yl)phenoxy]fluroacetate as an oil, Compound 51.

Aufarbeitung

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 34 hours
  3. temperatureThe mixture was cooled
  4. customthe solvent was removed by evaporation under reduced pressure
  5. customleaving a residue
  6. washthe solution was washed first with water
  7. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customThe filtrate was evaporated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-a835f0198b834866b0ef1002e91602ab
Quelldatensatz
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04806145

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