Reacción #1336777

ord-6f219c6f9da04028b3b57e31293aec97

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawere heated
  2. 2
    Temperaturaat reflux overnight
  3. 3
    Temperaturathe mixture was refluxed for 2 hours
  4. 4
    Temperaturacooled
  5. 5
    FiltraciónThe resulting brown solid was filtered
  6. 6
    Lavadowashed with water until the washings
  7. 7
    Filtraciónfiltered
  8. 8
    Lavadowashed with ethanol and hexane
  9. 9
    Otrodried in vacuo

Procedimiento

A mixture of 2-(hydroxymethyl)-5-[(phenylmethyl)oxy]-4H-pyran-4-one (9.65 g, 41.59 mmole), 95 ml of concentrated ammonia and 20 ml of ethanol were heated at reflux overnight. An additional 75 ml of ammonium hydroxide was added, the mixture was refluxed for 2 hours and cooled. The resulting brown solid was filtered and washed with water until the washings were neutral. The crude product was suspended in ethanol, filtered, washed with ethanol and hexane and dried in vacuo. The yield of the title compound was 7.61 g.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04632985uspto-grants-1986_12