Reaktion #94870

ord-80e63a5c163a4426b44a1d8406a739fb

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxed for 15 minutes
  2. 2
    Temperaturthe acidified mixture refluxed for 15 minutes
  3. 3
    SonstigeIncomplete reaction
  4. 4
    Temperaturthe mixture refluxed another 15 minutes
  5. 5
    Temperaturcooled
  6. 6
    Sonstigeevaporated to dryness

Vorschrift

1-Phenylpyrrole (1.4 g., 0.01 mole), alloxan hydrate (1.6 g., 0.01 mole) and 50 ml. of ethanol were combined and refluxed for 15 minutes. No reaction was noted by tlc. 1 N Hydrochloric acid (10 ml., 0.01 mole) was added and the acidified mixture refluxed for 15 minutes. Incomplete reaction was noted by tlc. A second portion of alloxan hydrate (1.6 g., 0.01 mole) was added and the mixture refluxed another 15 minutes, cooled and evaporated to dryness. Trituration of the residue with water gave title product [2.3 g.; m/e 285; m.p. 232°-234° C. (dec); Rf 0.3 (1:1 ethyl acetate:hexane)].

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04342771uspto-grants-1982_08