Reacción #1049547

ord-65b8cf1f5b3045fb855b479b47c7a633

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónThe crystals were filtered off
  2. 2
    Otrocrystallized from ethanol
  3. 3
    OtroThe second fraction of the crystallization
  4. 4
    Otrowas recrystallized from ethanol

Procedimiento

(±)-[2R*[1S*,5S*(S*)]]+[2R*[1S*,5R*(R*)]]-α,α'[iminobis(methylene)]bis[6-fluoro-3,4-dihydro-2H-1-benzopyran-2-methanol] (142 g) was converted into the hydrochloric acid salt in ethanol (1000 ml). The crystals were filtered off and crystallized from ethanol. The second fraction of the crystallization was recrystallized from ethanol, yielding 10.3 g (6.6%) of (±)-[2R*[1S*,5S*(S*)]]-α,α'[iminobis(methylene)]bis[6-fluoro-3,4-dihydro-2H-1-benzopyran-2-methanol]hydrochloride; mp. 224.9° C. nebivolol hydrochloride (crystalline compound 1).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05759580uspto-grants-1998_06