Water → bis(4-oxo-2-phenyl-4H-chromen-3-yl)terephthalate

HRID 1868535

Reaktionsgleichung

[OH:1][C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[O:4][C:3]=1[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[C:19](Cl)(=[O:29])[C:20]1[CH:28]=[CH:27][C:23]([C:24](Cl)=[O:25])=[CH:22][CH:21]=1.ClCCl.C(N([CH2:39][CH3:40])CC)C.[OH2:41]>>[C:19]([O:29][C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[O:4][C:3]=1[C:40]1[CH:39]=[CH:18][CH:13]=[CH:14][CH:15]=1)(=[O:41])[C:20]1[CH:28]=[CH:27][C:23]([C:24]([O:1][C:2]2[C:11](=[O:12])[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[O:4][C:3]=2[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)=[O:25])=[CH:22][CH:21]=1

Komponenten

Edukt 5

HCID 962Water

HCID 6344Dichloromethane

HCID 7488Terephthaloyl chloride

HCID 8471Triethylamine

HCID 11349Flavonol

Produkt 1

HCID 57983717bis(4-oxo-2-phenyl-4H-chromen-3-yl)terephthalate

Versuchsvorschrift

To the three-necked round bottom flask attached with reflux condenser, calcium chloride guard tube and nitrogen inlet, 3-hydroxy-2-phenyl-4H-chromen-4-one (0.59 g), terephthaloyl chloride (0.59 g) and dichloromethane (50 ml) were charged. Then triethyl amine (0.29 g) was charged and the reaction mixture was stirred at room temperature and monitored by thin layer chromatography (TLC). On completion of the reaction 10 ml water was added to the reaction mixture and the organic layer was separated. The organic layer was dried and evaporated under reduced pressure to give the product.

Aufarbeitung

temperaturewith reflux condenser, calcium chloride guard tube and nitrogen inlet
additionwas added to the reaction mixture
customthe organic layer was separated
customThe organic layer was dried
customevaporated under reduced pressure
customto give the product

Quellen und Nachweise

ORD-Eintrag: ord-27ddcee096b342339cace111a5ba3e6b
Quelldatensatz: uspto-grants-2009_12
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07635778B2

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