反応 #3743

反応方程式

tert-butyl alcohol

sulfuric acid

2-cyanopyrazine

sodium hydroxide

→

N-tert-butyl-2-pyrazine-carboxamide

溶媒

water

反応条件

後処理

1. 1
   その他at 40° C. or less
2. 2
   その他at 9° to 15° C.
3. 3
   workup.WAITFurther, the temperature was kept at the same temperature for 2.5 hours
4. 4
   その他After the reaction
5. 5
   その他the reaction liquid
6. 6
   workup.STIRRINGwith stirring
7. 7
   その他Precipitated crystalline solid was separated by filtration
8. 8
   洗浄washed with water
9. 9
   その他dried

実験手順

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.

出典