Reaktion #155899

ord-5477a329b1b04fd7853d9aa383ddd7bd

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeInto a 250-mL 3-necked round-bottom flask, was placed
  2. 2
    Sonstigeat room temperature
  3. 3
    Sonstigeat room temperature
  4. 4
    Sonstigeat room temperature
  5. 5
    TemperaturThe resulting solution was heated
  6. 6
    Temperaturto reflux for 3 hr
  7. 7
    EinengenThe resulting mixture was concentrated under vacuum
  8. 8
    Temperaturcooled with a water/ice bath
  9. 9
    FiltrationThe solids were collected by filtration

Vorschrift

Into a 250-mL 3-necked round-bottom flask, was placed malononitrile (20.4 g, 309.09 mmol, 1.00 equiv) at room temperature. To the resulting mixture was then added 1,1,1-triethoxyethane (50 g, 308.64 mmol, 1.00 equiv), in portions at room temperature. To the resulting mixture was then added acetic anhydride (72 g, 705.88 mmol, 2.28 equiv), in portions at room temperature. The resulting solution was heated to reflux for 3 hr. The resulting mixture was concentrated under vacuum, then cooled with a water/ice bath. The solids were collected by filtration to yield 2-(1-ethoxyethylidene)malononitrile as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822447B2uspto-grants-2014_09