Reaktion #59443

Reaktionsgleichung

piperidine

Malononitrile

2-fluorobenzaldehyde

→

title material

Ausbeute 28.3%

2-(2-Fluoro-benzylidene)-malononitrile

Ausbeute 28.3%

Lösungsmittel

iso-propyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewere placed in a vessel
2. 2
   Sonstigewhich was irradiated in a 300 W single mode microwave for 15 seconds
3. 3
   Filtrationfiltered
4. 4
   Sonstigeevaporated
5. 5
   Filtrationfiltered through a pad of Magnasol
6. 6
   Sonstigeevaporated
7. 7
   Sonstigerecrystallized from ethanol

Vorschrift

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,

Quelle