反応 #95547

反応方程式

trimethyl phosphite

2-iodomethyl-3-iodopropene

trimethyl phosphite

→

title compound

収率 92.0%

1,3-bis(dimethylphosphono)-2-methylene-propane

収率 92.0%

溶媒

benzene

反応条件

後処理

1. 1
   その他equipped with an addition funnel, a gas inlet tube
2. 2
   workup.DISTILLATIONa Vigreux column with distilling head
3. 3
   温度The phosphite was heated
4. 4
   温度at reflux
5. 5
   その他to collect
6. 6
   workup.DISTILLATIONDistillation of the reaction mixture

実験手順

400 ml of trimethyl phosphite was placed into a 2-1 flask equipped with an addition funnel, a gas inlet tube, and a Vigreux column with distilling head. The phosphite was heated at reflux, then a solution of 131 g (0.425 Mole) of 2-iodomethyl-3-iodopropene [see J.Amer.Chem.Soc., 89, 4688 (1967)] in 200 ml of benzene was added dropwise over a period of 2 h, followed by an additional 100 ml of trimethyl phosphite within 30 min. The reaction was run under nitrogen, and approx. 150 ml of distillate was allowed to collect. Distillation of the reaction mixture afforded 106 g (92%) of the title compound, b.p. 125°-7°/0.08 Torr;

出典