Reaktionsgleichung
[CH3:1][O:2][C:3](=[O:8])[CH2:4][N+:5]([O-:7])=[O:6].[CH:9](OCC)(OCC)[O:10][CH2:11][CH3:12].C(OC(=O)C)(=O)C>>[CH3:1][O:2][C:3](=[O:8])[C:4]([N+:5]([O-:7])=[O:6])=[CH:9][O:10][CH2:11][CH3:12]Komponenten
4
Versuchsvorschrift
A 12-1. three-necked flask, equipped with a thermometer, mechanical stirrer and a reflux condenser was charged under an atmosphere of nitrogen with 746 g (6.26 moles) of nitroacetic acid methylester, 1392 g (9.4 moles) of triethyl orthoformate and 1.92 l of acetic anhydride. The mixture was stirred and heated at reflux for 23 hours. The volatile components were distilled off first at atmospheric pressure (pot temperature up to 100° C., then at aspirator vacuum and finally at 0.17 mmHg (pot temperature up to 70°), leaving 926 g (84%) of crude alpha-nitro-beta-ethoxyacrylic acid methylester as an orange oil.
Aufarbeitung
- customthree-necked flask, equipped with a thermometer, mechanical stirrer and a reflux condenser
- temperatureheated
- temperatureat reflux for 23 hours
- distillationThe volatile components were distilled off first at atmospheric pressure (pot temperature up to 100° C.
Quellen und Nachweise
- ORD-Eintrag
- ord-f4cc5be488af4ae89d3ca1bd70b19add
- Quelldatensatz
- uspto-grants-1981_03
- Patentnummer
- US04256641
Verknüpfte Notizen
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