반응 #350451

ord-8a9e175df9cb4304ad949abc9a2e514c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooling the mixture
  2. 2
    workup.ADDITIONthe mixture is poured on to ice
  3. 3
    기타the organic phase is decanted
  4. 4
    세척washed with water and dilute hydrochloric acid
  5. 5
    건조dried over sodium sulphate
  6. 6
    workup.DISTILLATIONAfter distillation under vacuum (123° C.-125° C. and 0.4 mm. Hg) the title comound
  7. 7
    기타is obtained

실험 절차

300 g. of tetraethylene glycol and 100 g. of anhydrous pyridine are slowly added to 727 g. of phosphorus tribromide, while agitating and cooling the mixture. After cooling to room temperature, the mixture is poured on to ice and the organic phase is decanted, washed with water and dilute hydrochloric acid and dried over sodium sulphate. After distillation under vacuum (123° C.-125° C. and 0.4 mm. Hg) the title comound is obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04156683uspto-grants-1979_05