Reacción #570149

ord-87799a5586e54577b601993e30d2f3cd

Ecuación de reacción

N=C(N)NN.O=C(O)O
aminoguanidine bicarbonate
CC(=O)C1CCOC1=O
2-acetyl butyrolactone
Cc1nc(N)n(N)c(=O)c1CCO
desired intermediate
Rendimiento 65.2%
Cc1nc(N)n(N)c(=O)c1CCO
2,3-Diamino-5-(2-hydroxyethyl)-6-methyl-4(3H)-pyrimidinone
Rendimiento 65.2%

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawas heated
  2. 2
    Temperaturaat reflux until a clear solution
  3. 3
    Otrowas obtained
  4. 4
    TemperaturaThis solution was cooled
  5. 5
    Otroevaporated to dryness in vacuo
  6. 6
    Otrothe residue was triturated with 200 ml of a 50/50 ether-chloroform mixture

Procedimiento

A mixture of 13.6 g of aminoguanidine bicarbonate and 12.8 g of 2-acetyl butyrolactone in 80 ml of n-butanol was heated at reflux until a clear solution was obtained. This solution was cooled, evaporated to dryness in vacuo and the residue was triturated with 200 ml of a 50/50 ether-chloroform mixture, giving 12 g of the desired intermediate, mp 126°-135° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04577018uspto-grants-1986_03