Sulfuric Acid → 1-Aminocyclohexanecarboxamide

HRID 328365ノート

反応式

HRID 328365 の反応式
S(=O)(=O)(O)O.[NH2:6][C:7]1([C:13]#[N:14])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1.[OH-:15].[Na+]>>[NH2:6][C:7]1([C:13]([NH2:14])=[O:15])[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]1

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 14798Sodium HydroxideHCID 796351-Aminocyclohexanecarbonitrile

生成物 1

HCID 112405481-Aminocyclohexanecarboxamide

反応条件

温度
100 °C

実験手順

To 20 g concentrated sulfuric acid at 5° C is added with stirring 10 g of 1-aminocyclohexanecarbonitrile. After the addition, the mixture is heated with stirring at 100° C for 1 hour. The hot solution is then poured onto ice, the solution made strongly basic with 50% aqueous sodium hydroxide solution, and extracted three times with chloroform. The extract is washed with water, saturated NaHCO3 solution, dried, and the solvent removed in vacuo to leave the product, 1-aminocyclohexanecarboxamide, as a crystalline residue, melting point 99°-102° C. This can be recrystallized from either benzene or ether to give a pure product, melting point 101°-102° C.

後処理

  1. additionAfter the addition
  2. temperaturethe mixture is heated
  3. additionThe hot solution is then poured onto ice
  4. extractionextracted three times with chloroform
  5. washThe extract is washed with water, saturated NaHCO3 solution
  6. customdried
  7. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-3f0beffc39e1416b9e605d744d30c323
出典データセット
uspto-grants-1977_04
特許番号
US04017510

反応ノート

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