Hydrochloric Acid → Ethyl 6-acetyl-1,4-benzodioxin-2-carboxylate

HRID 37155Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 37155
[Cl-].[Al+3].[Cl-].[Cl-].[C:5](Cl)(=[O:7])[CH3:6].[O:9]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[O:12][CH:11]=[C:10]1[C:19]([O:21][CH2:22][CH3:23])=[O:20].Cl>C(=S)=S>[C:5]([C:17]1[CH:16]=[CH:15][C:14]2[O:9][C:10]([C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:11][O:12][C:13]=2[CH:18]=1)(=[O:7])[CH3:6]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 10987416Ethyl 1,4-benzodioxin-2-carboxylate

Produkt 1

HCID 11806994Ethyl 6-acetyl-1,4-benzodioxin-2-carboxylateAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6348Carbon DisulfideLösungsmittel

Versuchsvorschrift

Slowly add 8.1 g (60.7 mmol) of aluminium chloride to a solution of 2.85 g (36.3 mmol) of acetyl chloride and 5 g (24.7 mmol) of ethyl 1,4-benzodioxin-2-carboxylate in 120 cm3 of carbon disulfide at 0° C. Stir for 4 hours at room temperature and then, after acid hydrolysis with 20 cm3 of 2N hydrochloric acid, extract the reaction mixture with methylene chloride. After drying the methylene chloride phase over magnesium sulfate, concentrating to dryness and washing with ethanol, ethyl 6-acetyl-1,4-benzodioxin-2-carboxylate is obtained in a yield of 95%.

Aufarbeitung

  1. customat 0° C
  2. extractionextract the reaction mixture with methylene chloride
  3. dry with materialAfter drying the methylene chloride phase over magnesium sulfate
  4. concentrationconcentrating to dryness
  5. washwashing with ethanol

Quellen und Nachweise

ORD-Eintrag
ord-130b5d40694543cea4acdd66c99fbeab
Quelldatensatz
uspto-grants-1995_05
Patentnummer
US05420132

Notizen zur Reaktion

Wird geladen…