反応 #54441

反応方程式

benzyl chloromethyl sulfide

triethylphosphite

→

title compound

Diethyl(benzylthiomethyl)phosphonate

反応条件

後処理

1. 1
   その他prepared
2. 2
   温度was heated
3. 3
   温度The temperature of the oil bath was then raised to 170° C.
4. 4
   その他the volatile materials removed by distillation under reduced pressure
5. 5
   その他The residue was chromatographed on silica
6. 6
   洗浄by eluting with ethyl acetate/benzene mixtures which
7. 7
   その他gave 21.5 g

実験手順

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.

出典