Reaktion #938093

Reaktionsgleichung

water

ethyl cyanoacetate

sodium

trichloroacetamidine

→

6-Amino-4-Hydroxy-2-Trichloromethylpyrimidine

Ausbeute 71.0%

Lösungsmittel

acetic acid

methanol

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe solution was refluxed 1 hour
2. 2
   Sonstigethe solvent was removed under rotary evaporation
3. 3
   Sonstigeto give a red paste
4. 4
   workup.DISSOLUTIONThis was dissolved in 20 ml
5. 5
   workup.ADDITIONwas added
6. 6
   Sonstigeto precipitate
7. 7
   FiltrationFiltration
8. 8
   Waschenwashing
9. 9
   Sonstigedrying of the product
10. 10
    Sonstigegave 16.1 g (71% yield

Vorschrift

To a solution of 5.8 g (0.025 g atom) sodium in 150 ml methanol at 15° C. was added 11.5 g (0.1 mole) trichloroacetamidine. To this was added 11.5 g (0.1 mole) ethyl cyanoacetate in 100 ml methanol. The solution was refluxed 1 hour and then the solvent was removed under rotary evaporation to give a red paste. This was dissolved in 20 ml warm water and 100 ml of 50% aqueous acetic acid was added, causing product to precipitate. Filtration, washing, and drying of the product gave 16.1 g (71% yield; mp 225°-230° C. (decomposed). The structure was confirmed via infrared and elemental analysis.

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