Acetic Anhydride → Ethyl 2-butyryl-3-ethoxyacrylate

Reaktionsgleichung

[C:1]([CH2:6][C:7]([O:9][CH2:10][CH3:11])=[O:8])(=[O:5])[CH2:2][CH2:3][CH3:4].[C:12]([O:15][C:16](=O)C)(=O)[CH3:13].C(OC(OCC)OCC)C>>[CH2:12]([O:15][CH:16]=[C:6]([C:1](=[O:5])[CH2:2][CH2:3][CH3:4])[C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH3:13]

Komponenten

Edukt 3

HCID 7918Acetic Anhydride

HCID 31214Ethyl orthoformate

HCID 238498Ethyl 3-oxohexanoate

Produkt 1

HCID 3359484Ethyl 2-butyryl-3-ethoxyacrylate

Versuchsvorschrift

A mixture of ethyl butyrylacetate (105.1 g), acetic anhydride (126 ml) and triethylorthoformate (117 ml) was stirred and boiled under reflux for 1.5 hours. The low boiling materials were distilled off under reduced pressure and the residue distilled under high vacuum to give ethyl 2-(ethoxymethylene)-3-oxohexanoate, b.p. 109°-120° C. (0.4 mmHg).

Aufarbeitung

temperatureunder reflux for 1.5 hours
distillationThe low boiling materials were distilled off under reduced pressure
distillationthe residue distilled under high vacuum

Quellen und Nachweise

ORD-Eintrag: ord-8469f7fe2b9a4676828fda6c5a3ef9f1
Quelldatensatz: uspto-grants-1995_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05464781

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