Reaktion #2168844
ord-b0059139f6444ac288023b6b0bcebe8a
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThe mixture was refluxed for 1 hour
- 2Temperaturto cool
- 3Filtrationfiltered
- 4Waschenwashed with dioxane/water (1:1, 20 mL)
- 5Trocknenwater (50 mL), and dried in vacuo
- 6SonstigeThe solid was recrystallized from chloroform
- 7Sonstigeto 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.