反応式
S(=O)(=O)(O)O.[C:6]([C:8]1[CH:13]=[N:12][CH:11]=[CH:10][N:9]=1)#[N:7].[C:14](O)([CH3:17])([CH3:16])[CH3:15].[OH-:19].[Na+]>O>[C:14]([NH:7][C:6]([C:8]1[CH:13]=[N:12][CH:11]=[CH:10][N:9]=1)=[O:19])([CH3:17])([CH3:16])[CH3:15]参加物
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. Therefore, the yield of N-tert-butyl-2-pyrazinecarboxamide obtained here was 91.9%.
後処理
- customat 40° C. or less
- customat 9° to 15° C.
- waitFurther, the temperature was kept at the same temperature for 2.5 hours
- customAfter the reaction
- customthe reaction liquid
- stirringwith stirring
- customPrecipitated crystalline solid was separated by filtration
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-9fdadf8460a44268ad330e47232344a9
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05922873
関連ノート
読み込み中…