Reaktion #56518

ord-1f75bfc4a18549a383df5e6ba879eded

Reaktionsgleichung

CC(=O)O.O=Cc1coc2ccc3ccc(O)cc3c2c1=O
9-hydroxy-1-oxo-1H-naphtho[2,1-b]pyran-2-carboxaldehyde acetate
Cl.NO
hydroxylamine hydrochloride
O=C[O-].[Na+]
sodium formate
N#Cc1coc2ccc3ccc(O)cc3c2c1=O
9-Hydroxy-1-oxo-1H-naphtho[2,1-b]pyran-2-carbonitrile

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis refluxed for 30 hrs
  2. 2
    SonstigeThe product crystallize
  3. 3
    Temperaturon cooling
  4. 4
    Filtrationis filtered
  5. 5
    Waschenwashed with acetone

Vorschrift

A mixture of 9-hydroxy-1-oxo-1H-naphtho[2,1-b]pyran-2-carboxaldehyde acetate (1 mm), hydroxylamine hydrochloride (1.3 mm) and sodium formate (2 mm) is refluxed for 30 hrs. in formic acid (3 parts). The product crystallize on cooling, is filtered and washed with acetone. The dry crystals are light beige, m.p. 289°-92° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04225722uspto-grants-1980_09