Reaktion #218238

Reaktionsgleichung

ethanol

guanidine carbonate

ethyl acetoacetate

→

2-Amino-6-Methyl-4-Pyrimidone

Ausbeute 68.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe above compound was prepared
2. 2
   Temperaturafter which heat
3. 3
   Temperaturthe mixture refluxed for 15 hours
4. 4
   Sonstigeprecipitation of the product
5. 5
   FiltrationSubsequent vacuum filtration
6. 6
   Waschenwashing with cold acetone

Vorschrift

The above compound was prepared according to a literature method (Hirschberg, J. H. K., Beijer, F. H., van Aert, H. A., Magusin, P. C. M., Sijbesma, R. P., Meijer, E. W., Macromolecules, 1999, 32, 2696-2705, the disclosure of which is totally incorporated herein by reference). To a 1 liter round bottom flask under an inert argon atmosphere was added 650 milliliters of dry ethanol and 90.08 grams (0.5 mole) of guanidine carbonate. Thereafter, with good stirring was added dropwise over 2 hours 130.17 grams (1 mole) of ethyl acetoacetate, after which heat was applied and the mixture refluxed for 15 hours. The mixture was then cooled to room temperature and 800 milliliters of deionized water was slowly added to induce precipitation of the product. Subsequent vacuum filtration and washing with cold acetone secured the anticipated product in 68 percent yield (mp 311° C.). All physical properties were in accord with the reported properties.

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