Réaction #48489
ord-c0ebcf4a032d459780495542121a9694
Équation de réaction
Réactifs
Aucun
Conditions de réaction
Conditions détaillées
See reaction.notes.procedure_details.
Traitement
- 1Autrethe volatiles were removed in vacuo
- 2workup.ADDITION500 ml of ethyl ether was added to the residue and insoluble solid
- 3Filtrationwas filtered away
- 4AutreConcentration of the filtrate and final removal of volatiles
Mode opératoire
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.