Reacción #161804

ord-a713b8b762d3463ca804602f6597b9ec

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThen the reaction mixture was evaporated down
  2. 2
    Otrothe rotary evaporator
  3. 3
    Temperaturarefluxed for a further 3 days
  4. 4
    FiltraciónThe solid was filtered off
  5. 5
    Otrothe filtrate evaporated down i
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in DMF
  7. 7
    Otropurified by preparative HPLC

Procedimiento

110 mg (0.43 mmol) (4-chloro-pyridin-2-yl)-(2,3-dihydro-indol-1-yl)-methanone, 150 mg (1.0 mmol) potassium carbonate and 100 mg (0.41 mmol) 3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one in 10 mL THF were refluxed for 3 days. Then the reaction mixture was evaporated down using the rotary evaporator, taken up in 20 mL xylene and refluxed for a further 3 days. The solid was filtered off and the filtrate evaporated down i. vac. The residue was dissolved in DMF and purified by preparative HPLC. The product fractions were combined and lyophilised.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08829006B2uspto-grants-2014_09