Reaktion #62744

Reaktionsgleichung

sodium methoxide

7,8-dimethoxy-5-formyl-2H-1-benzopyran

3-ethoxypropanenitrile

→

amber oil

Ausbeute 73.6%

3-(7,8-Dimethoxy-2H-1-benzopyran-5-yl)-2-methoxymethylpropenenitrile

Ausbeute 73.6%

Lösungsmittel

water

ethylether

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturat reflux for 4 hr
3. 3
   Temperaturto cool
4. 4
   SonstigeThe layers were separated
5. 5
   Waschenthe ether portion was washed with water (3×250 mL and 1×100 mL)
6. 6
   Trocknendried over magnesium sulfate
7. 7
   EinengenThe ether solution was concentrated

Vorschrift

A mixture of sodium methoxide (7.02 g, 0.13 mole), 7,8-dimethoxy-5-formyl-2H-1-benzopyran (57 g, 0.26 mole) and 3-ethoxypropanenitrile (28.35 g, 0.286 mole) in methanol (150 mL) was heated at reflux for 4 hr, allowed to cool and diluted with water (150 mL) and ethylether (500 mL). The layers were separated and the ether portion was washed with water (3×250 mL and 1×100 mL) and dried over magnesium sulfate. The ether solution was concentrated to give 55 g (73%) of an amber oil which was used without further purification.

Quelle