Acetic Acid → Methyl 3-(3,5-dimethoxyphenyl)-2-(4-isopropyloxyphenyl)-3-oxopropionate

HRID 424030

Reaktionsgleichung

[H-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([O:15][CH3:16])[CH:14]=1)[C:8]([O:10]C)=O.[CH:17]([O:20][C:21]1[CH:26]=[CH:25][C:24]([CH2:27][C:28]([O:30][CH3:31])=[O:29])=[CH:23][CH:22]=1)([CH3:19])[CH3:18].C(O)(=O)C>C1(C)C=CC=CC=1.O>[CH3:16][O:15][C:13]1[CH:12]=[C:7]([C:8](=[O:10])[CH:27]([C:24]2[CH:25]=[CH:26][C:21]([O:20][CH:17]([CH3:19])[CH3:18])=[CH:22][CH:23]=2)[C:28]([O:30][CH3:31])=[O:29])[CH:6]=[C:5]([O:4][CH3:3])[CH:14]=1

Komponenten

Reaktionsbedingungen

Temperatur: 2.5 °C

Versuchsvorschrift

14.4 g of 60% sodium hydride in mineral oil (0.36 mol) which are washed with 2 times 50 ml of toluene are introduced into a three-necked round-bottomed flask. 90 ml of toluene and 28.3 g of methyl 3,5-dimethoxybenzoate (0.144 mol) are then introduced. The mixture is brought to reflux and a solution of 30 g of methyl p-isopropyloxyphenylacetate (0.144 mol) dissolved in 95 ml of toluene is added over 10 h. The mixture is maintained at reflux for 2 h. It is cooled to a temperature of 0-5° C. and a solution of glacial acetic acid (22.5 g, i.e. 0.374 mol) in 25 ml of toluene is added slowly. Then, at ambient temperature, 135 ml of water are added slowly.

Aufarbeitung

additionare introduced into a three-necked round-bottomed flask
temperatureto reflux
additionis added over 10 h
temperatureThe mixture is maintained
temperatureat reflux for 2 h

Quellen und Nachweise

ORD-Eintrag: ord-f134aec402f947f3b6994412ef96e865
Quelldatensatz: uspto-grants-2012_01
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08101804B2

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