Sulfuric Acid → 1-Aminocyclohexanecarboxamide

HRID 372353Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 372353
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

Komponenten

4

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-7628f567fa014fcc972a07c38a902bb8
Quelldatensatz
uspto-grants-1978_05
Patentnummer
US04090860

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