Reaktion #1287292

ord-8b2020c248a6462d810476b0578b7108

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe solution was refluxed for three hours
  2. 2
    SonstigeThe cooled reaction mixture
  3. 3
    Extraktionthe product was extracted into 1,1'-oxybisethane
  4. 4
    WaschenThe extract was washed with water, sodium carbonate solution and water
  5. 5
    Trocknenthen dried over sodium sulphate
  6. 6
    Sonstigeevaporated

Vorschrift

5H-Dibenz[b,g]oxocin-6(7H)-one (3 g - as prepared in B) was dissolved in a mixture of formic acid (3 ml) and methylformamide (12 ml) containing magnesium chloride hexahydrate (0.6 g), and the solution was refluxed for three hours. The cooled reaction mixture was diluted with water and neutralised with sodium carbonate solution, then the product was extracted into 1,1'-oxybisethane. The extract was washed with water, sodium carbonate solution and water then dried over sodium sulphate, and evaporated to give 6,7-Dihydro-N-methyl-5H-dibenz[b,g]oxocine-6-formamide.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04904688uspto-grants-1990_02