Réaction #91558

ord-98cdeda5309a4808822ec3f028b69177

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurethis was heated in a microwave at 110 C
  2. 2
    Extractionthis was extracted with DCM (2×30 ml)
  3. 3
    LavageThe combined organics were washed with brine
  4. 4
    Séchagedried over sodium sulphate
  5. 5
    Concentrationconcentrated in vacuo
  6. 6
    AutreThe crude product was purified through silica eluting with 0-45% ethyl acetate in hexane

Mode opératoire

Potassium tert-butoxide (0.132 g) in ethanol (4 ml) was stirred for 15 min before adding 1,1-dimethylethyl 7-(5-acetyl-2-{[(4-chloro-2-pyridinyl)methyl]oxy}phenyl)-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate, (0.4 g) and this was heated in a microwave at 110 C. for 1.5 h. Water (20 ml) was added to the cooled mixture and this was extracted with DCM (2×30 ml). The combined organics were washed with brine, dried over sodium sulphate and concentrated in vacuo. The crude product was purified through silica eluting with 0-45% ethyl acetate in hexane to give the title compound, 0.16 g

Source

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