تفاعل #95547

معادلة التفاعل

trimethyl phosphite

2-iodomethyl-3-iodopropene

trimethyl phosphite

→

title compound

المردود 92.0%

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

المردود 92.0%

المذيبات

benzene

ظروف التفاعل

المعالجة

1. 1
   أخرىequipped with an addition funnel, a gas inlet tube
2. 2
   workup.DISTILLATIONa Vigreux column with distilling head
3. 3
   درجة الحرارةThe phosphite was heated
4. 4
   درجة الحرارةat reflux
5. 5
   أخرىto collect
6. 6
   workup.DISTILLATIONDistillation of the reaction mixture

الإجراء التجريبي

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;

المصدر