Reaktion #2251979

ord-d9f38410e974456fae91fe365c2b2f8c

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe resulting suspension was heated at 80° under nitrogen for 19 hours
  2. 2
    SonstigeThe cooled reaction mixture
  3. 3
    Waschenwashed with water (4×250 ml)
  4. 4
    TrocknenThe organic layer was dried over anhydrous Na2SO4
  5. 5
    Sonstigeevaporated in vacuo

Vorschrift

To a solution of 3.02 g of cis-1,2,3,4,4a,9b-hexahydro-4a-phenyl-benzofuro[3,2-c]pyridine in 48 ml of dry dimethylformamide was added 3.6 g of anhydrous potassium carbonate and 0.982 g of chloroacetonitrile. The resulting suspension was heated at 80° under nitrogen for 19 hours. The cooled reaction mixture was diluted with 500 ml of ether and washed with water (4×250 ml). The organic layer was dried over anhydrous Na2SO4 and evaporated in vacuo to give 3.48 g (99.9%) of a gum, which crystallized on standing. A 0.35 g portion of this material was recrystallized from ethanol to afford 0.22 g of crystals, m.p. s 93°, 94°-96°.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04507306uspto-grants-1985_03