Reaktionsgleichung
[CH3:1][O:2][C:3](=[O:9])[CH2:4][C:5]([CH2:7][Cl:8])=[O:6].[CH3:10]OC(OC)OC>>[CH3:1][O:2][C:3](=[O:9])/[CH:4]=[C:5](/[O:6][CH3:10])\[CH2:7][Cl:8]Komponenten
Reaktionsbedingungen
- Temperatur
- 150 °C
Versuchsvorschrift
31.0 g (0.2 mol) of 4-chloroacetoacetic acid methyl ester is mixed with 106.0 g (1.0 mol) of orthoformic acid trimethyl ester. 30.0 g of Amberlyst-15 ion exchange resin is added under argon with stirring. Under vigorous formation of gas, the reaction temperature rises to 40° C. After 5 hours of stirring, no educt can any longer be detected in thin-layer chromatography. It is filtered from the ion exchange resin and the residue is distilled in a water jet vacuum. The distillate is mixed with 1.0 g of p-toluene sulfonic acid monohydrate and slowly heated to 150° C., and methanol is distilled off. The reaction mass is then distilled in a water jet vacuum. 24.7 g of a colorless liquid with a boiling point bp12 =93° C. is obtained. Further data concerning the compound is:
Aufarbeitung
- addition30.0 g of Amberlyst-15 ion exchange resin is added under argon
- customrises to 40° C
- stirringAfter 5 hours of stirring
- filtrationIt is filtered from the ion exchange resin
- distillationthe residue is distilled in a water jet vacuum
- additionThe distillate is mixed with 1.0 g of p-toluene sulfonic acid monohydrate
- distillationmethanol is distilled off
- distillationThe reaction mass is then distilled in a water jet vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-5828ecdb379e40b292f004836af0e56a
- Quelldatensatz
- uspto-grants-1990_03
- Patentnummer
- US04906759
Verknüpfte Notizen
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