Реакция #48489

Уравнение реакции

bis-tert butyl phosphate

chloroiodomethane

→

di-tert-butyl chloromethyl phosphate

Условия реакции

Обработка

1. 1
   Другоеthe volatiles were removed in vacuo
2. 2
   workup.ADDITION500 ml of ethyl ether was added to the residue and insoluble solid
3. 3
   Фильтрацияwas filtered away
4. 4
   ДругоеConcentration of the filtrate and final removal of volatiles

Методика

The tetrabutylammonium salt of bis-tert butyl phosphate (57 g, 0.126 mol, Digital Specialty Chemicals) and chloroiodomethane (221 g, 1.26 mol) were stirred at room temperature for four hours and then the volatiles were removed in vacuo. 500 ml of ethyl ether was added to the residue and insoluble solid was filtered away. Concentration of the filtrate and final removal of volatiles using a vacuum pump provided di-tert-butyl chloromethyl phosphate (112 g), typically as a light yellow or brown oil, which was utilized in the next step without any further purification.

Источник