Reacción #51656

ord-fb291dc7b7414f87a6d19f68f18c6b15

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Otrothe reaction vessel is sealed
  2. 2
    workup.WAITIt is left
  3. 3
    workup.WAITto stand at about 20° C. for 3 weeks with the exclusion of light
  4. 4
    OtroThe solution is evaporated to dryness
  5. 5
    Otrothe residue is recrystallized from acetonitrile

Procedimiento

2.00 g (0.0048 mol) of 4.1 is dissolved in 20 ml dichloromethane and 20 ml acetonitrile, combined with 2.59 g (0.0238 mol) of bromoethane and the reaction vessel is sealed. It is left to stand at about 20° C. for 3 weeks with the exclusion of light. The solution is evaporated to dryness and the residue is recrystallized from acetonitrile. Yield: 1.96 g of 3 (78% of theory); TLC: Rf value: 0.11 (eluant as in step II.1); melting point: 247° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US06852728B2uspto-grants-2005_02