Reacción #1177768

ord-2c674c8da3f34779851e966d67b57d19

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Lavadothe ethyl acetate layer was sequentially washed with water
  2. 2
    Secadoa saturated sodium chloride aqueous solution twice in each case, and dried over magnesium sulfate
  3. 3
    FiltraciónThe solution was filtered
  4. 4
    Otroevaporated under a reduced pressure
  5. 5
    Otroresulting residue
  6. 6
    Otrowas purified on a silica gel column (silica gel 50 g, eluant: 5% methanol in chloroform)

Procedimiento

1.31 g of t product of Example 172 was dissolved in 3 ml of dimethylformamide, to the solution were added 644 mg of 1,2-dibromoethane and 1.13 g of anhydrous potassium carbonate at a room temperature, and the mixture was stirred for 24 hours. After adding 100 ml of ethyl acetate, the ethyl acetate layer was sequentially washed with water and a saturated sodium chloride aqueous solution twice in each case, and dried over magnesium sulfate. The solution was filtered and evaporated under a reduced pressure, and resulting residue was purified on a silica gel column (silica gel 50 g, eluant: 5% methanol in chloroform), to obtain 356 mg of the title compound in a colorless amorphous form, while recovering the residual starting material.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05081246uspto-grants-1992_01