Triethylamine → HCID 54343021, Verbindung

HRID 1872397

Reaktionsgleichung

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

Komponenten

Reaktionsbedingungen

Temperatur: 0 °C

Versuchsvorschrift

To a solution of titanium(IV) chloride (13.88 g) in dichloromethane (100 ml) was added Ethyl 4-acetylbenzoate (11.53 g) and 4-n-pentyloxybenzaldehyde (12.68 g) in dichloromethane (50 ml) was added dropwise at 0° C. To the mixture was added triethylamine (12.44 ml) in dichloromethane (30 ml). The mixture was stirred at 0° C. for 30 minutes and diluted with ethyl acetate. The organic layer was washed with water (four times) and brine and dried over magnesium sulfate. The solvents were removed under reduced pressure and the residue was triturated with n-hexane. The solid was collected by filtration and dried to give 1-(4-n-Pentyloxyphenyl)-3-(4-ethoxycarbonylphenyl)-1-propen-3-one (13.45 g).

Aufarbeitung

additionwas added dropwise at 0° C
washThe organic layer was washed with water (four times) and brine
dry with materialdried over magnesium sulfate
customThe solvents were removed under reduced pressure
customthe residue was triturated with n-hexane
filtrationThe solid was collected by filtration
customdried

Quellen und Nachweise

ORD-Eintrag: ord-5929b187f2df40f981646c2892dd1128
Quelldatensatz: uspto-grants-2000_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06107458

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