반응 #42015

ord-bd280309d1274ad4b0b18844835c296f

반응 방정식

[Na+].[O-][Br+2]([O-])[O-]
sodium bromate
OCc1ccccc1
benzyl alcohol
CCOCC
ether
O=C(O)c1ccccc1
benzoic acid
수율 90.0%

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    여과the catalyst was filtered off
  3. 3
    기타The organic layer was separated
  4. 4
    추출the aqueous phase was extracted with ether (2×50 ml)
  5. 5
    세척The combined organic extracts were washed with water (25 ml)
  6. 6
    건조dried with anhydrous magnesium sulphate
  7. 7
    농축concentrated

실험 절차

A mixture of Ceiv catalyst from Example 47 (0.08 g), sodium bromate (0.3 g) and benzyl alcohol (0.216 g, 2 mmol) in acetonitrile:water (5:7, 12 ml) was stirred at 80° C. for 40 h under an atmosphere of nitrogen. On cooling ether (70 ml) was added and the catalyst was filtered off. The organic layer was separated and the aqueous phase was extracted with ether (2×50 ml). The combined organic extracts were washed with water (25 ml), dried with anhydrous magnesium sulphate and concentrated to give benzoic acid as a white solid (0.22 g, 90%). M.p. 120° C., lit. 120-122° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728159B2uspto-grants-2010_06