Reacción #5832

ord-06bb6720d27140e6bd8fead9cef0ffdf

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónextracted twice with 80 ml of chloroform
  2. 2
    SecadoThe extract was dried over magnesium sulfate
  3. 3
    Concentraciónconcentrated under a reduced pressure
  4. 4
    Otroresulting residue
  5. 5
    Lavadoeluted with chloroform/methanol (100:1)
  6. 6
    Otroresulting crystals
  7. 7
    Lavadowas washed with ethyl acetate

Procedimiento

4.52 g of the crystals obtained in Reference Example 41 was dissolved in 50 ml of pyridine, to the solution were added 5.8 g of 5-isoquinolinesulfonyl chloride hydrochloride and 3 g of dimethylaminopyridine, and the mixture was stirred for 18 hours at a room temperature, after adding 150 ml of water, extracted twice with 80 ml of chloroform. The extract was dried over magnesium sulfate and concentrated under a reduced pressure, and resulting residue was applied to a silica gel column and eluted with chloroform/methanol (100:1), and resulting crystals was washed with ethyl acetate, to obtain 1.2 g of the title compound as yellow crystals.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05245034uspto-grants-1993_09