Reacción #172500

ord-747163de371a4142b2f6a7dd3e0c992e

Disolventes

Condiciones de reacción

Temperatura
50°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe precipitate was separated by filtration
  2. 2
    Lavadowashed with methanol
  3. 3
    OtroThe crystal was purified by silica gel column chromatography
  4. 4
    Lavadowashed with methanol
  5. 5
    Otroto give 228 mg of a dark blue crystal
  6. 6
    Otroamp of 250-252° C. (yield: 85.2%)

Procedimiento

In 5 ml of ethanol were dissolved 150 mg (0.65 mmol) of 8-methoxy-2,3,6,7-tetrahydro-1H,5H-benzo[ij]quinolizine-9-carboaldehyde and 142 mg (0.71 mmol) of 2-(3-cyano-4,5,5-trimethyl-2(5H)-furanylidene)propanedinitrile. The mixture was stirred at room temperature for 3 hours and further at 50° C. for 3 hours. The precipitate was separated by filtration and washed with methanol. The crystal was purified by silica gel column chromatography and washed with methanol to give 228 mg of a dark blue crystal having amp of 250-252° C. (yield: 85.2%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08846955B2uspto-grants-2014_09