Reaktion #2168844

ord-b0059139f6444ac288023b6b0bcebe8a

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was refluxed for 1 hour
  2. 2
    Temperaturto cool
  3. 3
    Filtrationfiltered
  4. 4
    Waschenwashed with dioxane/water (1:1, 20 mL)
  5. 5
    Trocknenwater (50 mL), and dried in vacuo
  6. 6
    SonstigeThe solid was recrystallized from chloroform
  7. 7
    Sonstigeto yield 4.16 g, m.p. 147°-150° C.

Vorschrift

Cyanogen bromide (2.9 g, 0.027 mol) was added to a mixture of the compound prepared in Step 1 above (6.1 g, 0.025) and KHCO3 (2.8 g, 0.028 mol) in dioxane/water (1:1, 50 mL) at room temperature. The mixture was refluxed for 1 hour, allowed to cool, filtered, washed with dioxane/water (1:1, 20 mL), then water (50 mL), and dried in vacuo. The solid was recrystallized from chloroform to yield 4.16 g, m.p. 147°-150° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05185358uspto-grants-1993_02