Hydrochloric Acid → 3-Ethoxy-3-cyclobutene-1,2-dione
Reaktionsgleichung
C([O:3][C:4]1(OCC)[C:7](OCC)([O:8][CH2:9][CH3:10])[CH2:6][C:5]1=[O:14])C.Cl>>[CH2:9]([O:8][C:7]1[C:4](=[O:3])[C:5](=[O:14])[CH:6]=1)[CH3:10]Komponenten
3
Versuchsvorschrift
##STR7## 45 g of 2,2,3,3-tetraethoxycyclobutanone are stirred vigorously at 50° C in 4 normal aqueous HCl until the starting material is no longer detectable. The reaction solution is then extracted for 20 hours continuously with diethyl ether and the organic extracts are dried over MgSO4 and concentrated. Precipitated crystals of 1-hydroxycyclobutene-3,4-dione are filtered off sharply and the liquid residue is distilled at 110° C/0.1 Torr to yield 6.65 g (=30% of theory) of the desired 1-ethoxycyclobutene-3,4-dione of the above structure.
Aufarbeitung
- extractionThe reaction solution is then extracted for 20 hours continuously with diethyl ether
- dry with materialthe organic extracts are dried over MgSO4
- concentrationconcentrated
- customPrecipitated crystals of 1-hydroxycyclobutene-3,4-dione
- filtrationare filtered off sharply
- distillationthe liquid residue is distilled at 110° C/0.1 Torr
Quellen und Nachweise
- ORD-Eintrag
- ord-196e75bb90e24370bbfbc5dcc3c35dfa
- Quelldatensatz
- uspto-grants-1978_05
- Patentnummer
- US04092146
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