Sulfuric Acid → Diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate

HRID 486255

Reaktionsgleichung

Reaktionsgleichung von HRID 486255
[Mg].[C:2]([O:10][CH2:11][CH3:12])(=[O:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[CH3:13][C:14]1[C:22]([F:23])=[C:21]([F:24])[CH:20]=[C:19]([F:25])[C:15]=1[C:16](Cl)=[O:17].S(=O)(=O)(O)O>C(Cl)(Cl)(Cl)Cl.C(O)C.C1(C)C=CC=CC=1.O>[CH3:13][C:14]1[C:22]([F:23])=[C:21]([F:24])[CH:20]=[C:19]([F:25])[C:15]=1[C:16]([CH:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[C:2]([O:10][CH2:11][CH3:12])=[O:9])=[O:17]

Komponenten

9

Edukt 4

HCID 1118Sulfuric AcidHCID 7761Diethyl MalonateHCID 5462224MagnesiumHCID 150076072-Methyl-3,4,6-trifluorobenzoyl chloride

Produkt 1

HCID 17879412Diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 5943Carbon TetrachlorideKatalysatorHCID 702EthanolLösungsmittel2×HCID 962WaterLösungsmittelHCID 1140TolueneLösungsmittel2×

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

Separately, two drops of carbon tetrachloride are added to a solution of metallic magnesium (0.4 g) in absolute ethanol (0.9 ml). When the reaction starts, a mixture of diethyl malonate (2.6 ml), absolute ethanol (1.6 ml) and anhydrous toluene (6 ml) is added dropwise below 60° C. After stirring at 60° C. for 1 hour, the reaction mixture is cooled to 0° C. and thereto a solution of 2-methyl-3,4,6-trifluorobenzoyl chloride prepared above in toluene (5 ml) is added dropwise. After stirring for 30 minutes, a mixture of conc. sulfuric acid (0.4 ml) and water (6 ml) is added and the mixture is extracted with diethyl ether, and the extract is dried over magnesium sulfate and concentrated to give diethyl 2-methyl-3,4,6-trifluorobenzoylmalonate (5.2 g).

Aufarbeitung

  1. additionis added dropwise below 60° C
  2. temperaturethe reaction mixture is cooled to 0° C.
  3. additionis added dropwise
  4. stirringAfter stirring for 30 minutes
  5. additionis added
  6. extractionthe mixture is extracted with diethyl ether
  7. dry with materialthe extract is dried over magnesium sulfate
  8. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-000195313545411088a60b5fdbe38b46
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05290934

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