反応 #3744

反応方程式

tert-butyl alcohol

sulfuric acid

2-cyanopyrazine

sodium hydroxide

→

N-tert-butyl-2-pyrazinecarboxamide

溶媒

water

反応条件

後処理

1. 1
   その他at 40° C. or less
2. 2
   workup.WAITFurther, the temperature was kept at the same temperature for 2.5 hours
3. 3
   その他After that, the reaction liquid
4. 4
   workup.STIRRINGwith stirring
5. 5
   その他The precipitated crystalline solid was separated by filtration
6. 6
   洗浄washed with water
7. 7
   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 of which internal temperature was kept at 9° to 15° C. over 3 hours. Further, the temperature was kept at the same temperature for 2.5 hours. After that, the reaction liquid was poured into 3500 g of water with stirring. Thus obtained mixture was neutralized with an aqueous solution of sodium hydroxide. The precipitated crystalline solid was separated by filtration, washed with water and dried to obtain 338.7 g (1.89 moles) of N-tert-butyl-2-pyrazinecarboxamide. It had a melting point of 88° to 90° C. Further, from the filtrate 7.17 g (0.04 mole) of N-tert-butyl-2-pyrazine-carboxamide was further obtained by extraction thereof with toluene. The yield thereof was 91.9%.

出典