Sulfuric Acid → N-tert-butylpyrazine-2-carboxamide

HRID 582246

反応式

HRID 582246 の反応式
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

6

反応物 4

HCID 1118Sulfuric AcidHCID 6386tert-ButanolHCID 14798Sodium HydroxideHCID 73172Pyrazinecarbonitrile

生成物 1

HCID 4462842N-tert-butylpyrazine-2-carboxamide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 1030 g of an 80% aqueous solution of sulfuric acid (8.40 moles of sulfuric acid), 220.5 g (2.1.0 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%.

後処理

  1. customat 40° C. or less
  2. waitFurther, the temperature was kept at the same temperature for 2.5 hours
  3. customAfter that, the reaction liquid
  4. stirringwith stirring
  5. customThe precipitated crystalline solid was separated by filtration
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-67bfbf4fc3fa46f5a3ac06040410d88e
出典データセット
uspto-grants-1999_07
特許番号
US05922873

関連ノート

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