反応 #59443

ord-8e87faf475de4826847a48546c5fff7a

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他were placed in a vessel
  2. 2
    その他which was irradiated in a 300 W single mode microwave for 15 seconds
  3. 3
    ろ過filtered
  4. 4
    その他evaporated
  5. 5
    ろ過filtered through a pad of Magnasol
  6. 6
    その他evaporated
  7. 7
    その他recrystallized from ethanol

実験手順

Malononitrile (3.303 g, 50 mmol), 2-fluorobenzaldehyde (6.205 g, 50 mmol), 1 g of molecular sieves, and 500 mg of a resin bound piperidine (described in Tetrahedron Lett., 1999, 40, 7031-33) were placed in a vessel which was irradiated in a 300 W single mode microwave for 15 seconds. The reaction mixture was taken up in iso-propyl acetate, filtered, evaporated, taken up in dichloromethane, filtered through a pad of Magnasol, evaporated, and recrystallized from ethanol to yield 2.435 g of the title material as a crystalline solid,

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07425580B2uspto-grants-2008_09