반응 #172508

ord-aa904c33c98c433fa27ac7ea2aa63a45

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the precipitate was separated by filtration
  2. 2
    세척washed with water
  3. 3
    기타dried
  4. 4
    기타The crystal was purified by silica gel column chromatography
  5. 5
    세척washed with methanol

실험 절차

In 10 ml of anhydrous acetic acid were dissolved 0.8 g (3.04 mmol) of 4-(dibutylamino)-2-methoxybenzaldehyde and 0.73 g (3.01 mmol) of 1,3-bis(dicyanomethylidene)indan. The mixture was stirred with heating at 80° C. for 2 hours. The reaction mixture was poured into 200 ml of water and the precipitate was separated by filtration, washed with water, and dried. The crystal was purified by silica gel column chromatography and washed with methanol to give 1.27 g of a black crystal having a mp of 195-198° C. (yield: 86.4%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846955B2uspto-grants-2014_09