Reaktion #91563

ord-ad30594234a44bc1aa023133bea3df46

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeOn completion the solid formed
  2. 2
    Filtrationwas collected by filtration
  3. 3
    Waschenwashed with acetone
  4. 4
    workup.DISSOLUTIONThe solid was then dissolved in water
  5. 5
    SonstigeSolid was obtained which
  6. 6
    Filtrationwas collected by filtration
  7. 7
    SonstigeThis was triturated with diethyl ether

Vorschrift

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%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447074B2uspto-grants-2016_09