Dimethylformamide → Methyl 4-(4-oxo-4-phenylbutoxy)benzoate ethylene acetal

HRID 1585650

Reaktionsgleichung

Reaktionsgleichung von HRID 1585650
[C:1]1([C:7]2([CH2:12][CH2:13][CH2:14]Cl)OCC[O:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:16](=[O:19])([O-])[O-].[K+].[K+].[OH:22][C:23]1[CH:32]=[CH:31][C:26]([C:27]([O:29][CH3:30])=[O:28])=[CH:25][CH:24]=1.[CH3:33]N(C)C=O>O>[CH2:16]1[O:19][C:27]([O:28][CH3:33])([C:26]2[CH:25]=[CH:24][C:23]([O:22][CH2:14][CH2:13][CH2:12][C:7](=[O:8])[C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)=[CH:32][CH:31]=2)[O:29][CH2:30]1

Komponenten

6

Edukt 4

HCID 6228DimethylformamideHCID 7456MethylparabenHCID 11430Potassium CarbonateHCID 128663382-(3-Chloropropyl)-2-phenyl-1,3-dioxolane

Produkt 1

HCID 70111092Methyl 4-(4-oxo-4-phenylbutoxy)benzoate ethylene acetal

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Crude 2-phenyl-2-(3-chloropropyl)-1,3-dioxolane (21.0 g), potassium carbonate (14.0 g; 0.101 moles) and methyl 4-hydroxybenzoate (14.0 g, 0.092 moles) were heated in dimethylformamide (100 ml) for 21 hours. The mixture was diluted with water (250 ml) and extracted with dichloromethane (500 ml). The dichloromethane extract was washed with saturated sodium bicarbonate solution and then with water. The organic extract was concentrated in vacuo to give the product as a brown solid (27.3 g).

Aufarbeitung

  1. extractionextracted with dichloromethane (500 ml)
  2. extractionThe dichloromethane extract
  3. washwas washed with saturated sodium bicarbonate solution
  4. extractionThe organic extract
  5. concentrationwas concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-7132aa972471458f9d7cf03adf3145e6
Quelldatensatz
uspto-grants-1999_08
Patentnummer
US05939447

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