반응 #2006474
ord-a490d813b217424c8d2caee980af7025
반응 방정식
tetrabutylammonium di-tert-butyl phosphate
chloroiodomethane
→
di-tert-butyl chloromethyl phosphate
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타were removed under vacuum
- 2workup.ADDITION500 ml of ethyl ether was added to the residue and insoluble solid
- 3여과was filtered away
- 4기타Concentration of the filtrate in vacuo and removal of remaining volatiles
실험 절차
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.