Thionyl Chloride → 2-Chlorocarbonyl-6,11-dihydro-11-oxodibenz[b,e]oxepin

HRID 894192Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 894192
[O:1]=[C:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[CH2:6][O:5][C:4]2[CH:13]=[CH:14][C:15]([C:17]([OH:19])=O)=[CH:16][C:3]1=2.S(Cl)([Cl:22])=O>>[Cl:22][C:17]([C:15]1[CH:14]=[CH:13][C:4]2[O:5][CH2:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[C:2](=[O:1])[C:3]=2[CH:16]=1)=[O:19]

Komponenten

3

Edukt 2

HCID 24386Thionyl ChlorideHCID 12446821Olopatadine Impurity 17

Produkt 1

HCID 134560052-Chlorocarbonyl-6,11-dihydro-11-oxodibenz[b,e]oxepin

Versuchsvorschrift

Heat a solution of 5 gm. of 6,11-dihydro-11-oxodibenz[b,e]oxepin-2-carboxylic acid and 40 ml. of thionyl chloride under reflux for 20 minutes. Evaporate the reaction mixture under vacuum to dryness. Repeat the evaporation with two 30 ml. portions of carbon tetrachloride. Crystallize the residue from diisopropyl ether to obtain the title product.

Aufarbeitung

  1. temperatureHeat a solution of 5 gm
  2. customEvaporate the reaction mixture under vacuum to dryness
  3. customRepeat the evaporation with two 30 ml
  4. customCrystallize the residue from diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-03917c48796442249d1cb806af3c04d1
Quelldatensatz
uspto-grants-1981_08
Patentnummer
US04282365

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