Reaktionsgleichung
[C:1]([O:8]CC)(=[O:7])[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].C(OCC)(=O)C(OCC)=[O:13]>>[O:13]=[C:2]([CH2:3][CH2:4][CH2:5][CH3:6])[C:1]([OH:8])=[O:7]Komponenten
3
Versuchsvorschrift
Ethyl n-hexanoate and diethyl oxalate were subjected to Claisen condensation, and then hydrolyzed to form 2-oxo-n-hexanoic acid. This product was then condensed with diaminomaleonitrile to form 9.1 g (0.042 mole) of 2,3-dicyano-5-hydroxy-6-n-pentylpyrazine (m.p. 61°-64° C.). The product was dissolved in 120 g of phosphorus oxychloride, and 3.32 g (0.042 mole) of pyridine was added. The mixture was refluxed for 5 hours, and then worked up in the same way as in Example 3 and the resulting oily product was concentrated under reduced pressure. The resulting product was chromatographed on a silica gel column with benzene as an eluent to afford 6.0 g (yield 61%) of 2,3-dicyano-5-chloro-6-n-pentyl-pyrazine as a yellow liquid.
Quellen und Nachweise
- ORD-Eintrag
- ord-1cd0839dd27f4a348367a4e7dd8b5e04
- Quelldatensatz
- uspto-grants-1981_03
- Patentnummer
- US04259489
Verknüpfte Notizen
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