تفاعل #1049547

ord-65b8cf1f5b3045fb855b479b47c7a633

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe crystals were filtered off
  2. 2
    أخرىcrystallized from ethanol
  3. 3
    أخرىThe second fraction of the crystallization
  4. 4
    أخرىwas recrystallized from ethanol

الإجراء التجريبي

(±)-[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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05759580uspto-grants-1998_06