Reaktion #54441

Reaktionsgleichung

benzyl chloromethyl sulfide

triethylphosphite

→

title compound

Diethyl(benzylthiomethyl)phosphonate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeprepared
2. 2
   Temperaturwas heated
3. 3
   TemperaturThe temperature of the oil bath was then raised to 170° C.
4. 4
   Sonstigethe volatile materials removed by distillation under reduced pressure
5. 5
   SonstigeThe residue was chromatographed on silica
6. 6
   Waschenby eluting with ethyl acetate/benzene mixtures which
7. 7
   Sonstigegave 21.5 g

Vorschrift

A mixture of benzyl chloromethyl sulfide (20 g., 0.116 mole), prepared according to the method of Bohme, Fischer and Frank [Ann., 563, 54 (1949)], and triethylphosphite (26.9 g., 0.162 mole) was heated with stirring at 155° C. (bath temperature) for 8 hours under a nitrogen atmosphere. The temperature of the oil bath was then raised to 170° C. and the volatile materials removed by distillation under reduced pressure. The residue was chromatographed on silica by eluting with ethyl acetate/benzene mixtures which gave 21.5 g. of the title compound as a liquid.

Quelle