반응 #3743

반응 방정식

tert-butyl alcohol

sulfuric acid

2-cyanopyrazine

sodium hydroxide

→

N-tert-butyl-2-pyrazine-carboxamide

용매

water

반응 조건

후처리

1. 1
   기타at 40° C. or less
2. 2
   기타at 9° to 15° C.
3. 3
   workup.WAITFurther, the temperature was kept at the same temperature for 2.5 hours
4. 4
   기타After the reaction
5. 5
   기타the reaction liquid
6. 6
   workup.STIRRINGwith stirring
7. 7
   기타Precipitated crystalline solid was separated by filtration
8. 8
   세척washed with water
9. 9
   기타dried

실험 절차

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.

출처