Réaction #91563

ord-ad30594234a44bc1aa023133bea3df46

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreOn completion the solid formed
  2. 2
    Filtrationwas collected by filtration
  3. 3
    Lavagewashed with acetone
  4. 4
    workup.DISSOLUTIONThe solid was then dissolved in water
  5. 5
    AutreSolid was obtained which
  6. 6
    Filtrationwas collected by filtration
  7. 7
    AutreThis was triturated with diethyl ether

Mode opératoire

1,1-dimethylethyl 7-(5-acetyl-2-{[(4-methyl-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (3.0 g) was dissolved in dioxane (20 ml). Gaseous hydrogen chloride was passed through the reaction mixture for 1.5 h. The reaction was monitored by TLC. On completion the solid formed was collected by filtration and washed with acetone. The solid was then dissolved in water and the mixture neutralised with aqueous sodium hydroxide (1M). Solid was obtained which was collected by filtration. This was triturated with diethyl ether to yield the title compound, 2.1 g (88%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US09447074B2uspto-grants-2016_09