반응 #69599

ord-955a6e2a0d374c7495f12d087392dfcb

반응 조건

온도
-10°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe resulting mixture was stirred for 12 hr at room temperature
  2. 2
    기타The organic layer was separated
  3. 3
    추출the aqueous layer was extracted with 2×100 mL of water
  4. 4
    세척The combined organic extracts were washed with aqueous NaHCO3
  5. 5
    건조dried over Na2SO4
  6. 6
    기타evaporated to dryness

실험 절차

To a solution of 12.0 (60.5 mmol) of 1,2-diphenylethanol in 50 mL of dry diethyl ether, 11.0 g (3.80 mL, 40.0 mmol) of PBr3 was added with vigorous stirring at −10° C. The resulting mixture was stirred for 12 hr at room temperature and then added to 350 mL of cold water. The organic layer was separated, and the aqueous layer was extracted with 2×100 mL of water. The combined organic extracts were washed with aqueous NaHCO3, dried over Na2SO4, and evaporated to dryness. This procedure gave 13.2 g (84%) of the title product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08530593B2uspto-grants-2013_09