Reaktion #3743

Reaktionsgleichung

tert-butyl alcohol

sulfuric acid

2-cyanopyrazine

sodium hydroxide

→

N-tert-butyl-2-pyrazine-carboxamide

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeat 40° C. or less
2. 2
   Sonstigeat 9° to 15° C.
3. 3
   workup.WAITFurther, the temperature was kept at the same temperature for 2.5 hours
4. 4
   SonstigeAfter the reaction
5. 5
   Sonstigethe reaction liquid
6. 6
   workup.STIRRINGwith stirring
7. 7
   SonstigePrecipitated crystalline solid was separated by filtration
8. 8
   Waschenwashed with water
9. 9
   Sonstigedried

Vorschrift

To 1030 g of an 80% aqueous solution of sulfuric acid (8.40 moles of sulfuric acid), 220.5 g (2.10 moles) of 2-cyanopyrazine was added dropwise keeping the internal temperature at 40° C. or less with stirring. In succession, 187 g (2.52 moles) of tert-butyl alcohol was added dropwise to the mixture, keeping the internal temperature at 9° to 15° C., over 3 hours. Further, the temperature was kept at the same temperature for 2.5 hours. After the reaction, the reaction liquid was added to 3500 g of water with stirring. Thus obtained mixture was neutralized with an aqueous solution of sodium hydroxide. Precipitated crystalline solid was separated by filtration, washed with water and then dried to obtain 338.7 g (1.89 moles) of N-tert-butyl-2-pyrazine-carboxamide. It had a melting point of 88° to 90° C. Further, from the water layer, from which the intended product had been separated by filtration, 7.17 g (0.04 mole) of the intended product was further obtained by extraction thereof with toluene.

Quelle