Reaktion #48490
ord-56a2fca1e2d24473a6fdd37fbe0d53ca
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigewere removed under vacuum
- 2workup.ADDITION500 ml of ethyl ether was added to the residue and insoluble solid
- 3Filtrationwas filtered away
- 4SonstigeConcentration of the filtrate in vacuo and removal of remaining volatiles
Vorschrift
A mixture of tetrabutylammonium di-tert-butyl phosphate (57 g, 0.126 mol, Digital Specialty Chemicals) and chloroiodomethane (221 g, 1.26 mol) was stirred at room temperature for four hours before the volatiles were removed under vacuum. 500 ml of ethyl ether was added to the residue and insoluble solid was filtered away. Concentration of the filtrate in vacuo and removal of remaining volatiles using a vacuum pump provided di-tert-butyl chloromethyl phosphate as a light brown or yellow oil, which was utilized in the next step without further purification.