Reacción #549528

ord-30d619e8a99e4976ab7eadc900b6c30c

Disolventes

Condiciones de reacción

Temperatura
95°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    ConcentraciónThe mixture is then concentrated by evaporation to a volume of 50 ml
  2. 2
    Concentraciónthe cooled aqueous concentrate
  3. 3
    Extracciónis extracted three times with 100 ml of ethylene chloride each time
  4. 4
    SecadoThe organic phase is dried over magnesium sulfate
  5. 5
    Concentraciónconcentrated by evaporation
  6. 6
    OtroThe residue crystallises to thus yield 5 g of the title compound, m.p. 113°-115° C.

Procedimiento

15 g of guanidine carbonate are added to a mixture of 10 g of 1-cyclopropyl-butane-1,3-dione and 150 g of water, and stirring is maintained at 95° C. for 5 hours. The mixture is then concentrated by evaporation to a volume of 50 ml, and the cooled aqueous concentrate is extracted three times with 100 ml of ethylene chloride each time. The organic phase is dried over magnesium sulfate and concentrated by evaporation. The residue crystallises to thus yield 5 g of the title compound, m.p. 113°-115° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04515626uspto-grants-1985_05