Reaktion #346297

ord-e80aabcd89e34ccab2368d8b37109df6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis heated on the steam bath for 4 hr
  2. 2
    ExtraktionThe mixture is extracted with chloroform
  3. 3
    Waschenthe extracts are washed with sodium bicarbonate solution
  4. 4
    SonstigeThe organic solution is dried
  5. 5
    Sonstigeevaporated

Vorschrift

A mixture of 1,2,3a, 4,5,6-hexahydro-7,8-dimethoxypyrano[2,3,4-de]isoquinoline (10.0 g), described in Example 56, acetic anhydride (60.0 ml) and pyridine (0.5 ml) is heated on the steam bath for 4 hr. The mixture is poured into water and stirred for 2 hr. The mixture is extracted with chloroform and the extracts are washed with sodium bicarbonate solution and then with brine. The organic solution is dried and evaporated to leave the title compound. A sample, crystallized from isopropanol, had m.p. 100°- 102° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04036842uspto-grants-1977_07