تفاعل #42015

ord-bd280309d1274ad4b0b18844835c296f

الكواشف

المذيبات

ظروف التفاعل

درجة الحرارة
80°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    ترشيحthe catalyst was filtered off
  3. 3
    أخرىThe organic layer was separated
  4. 4
    استخلاصthe aqueous phase was extracted with ether (2×50 ml)
  5. 5
    غسيلThe combined organic extracts were washed with water (25 ml)
  6. 6
    تجفيفdried with anhydrous magnesium sulphate
  7. 7
    تركيزconcentrated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07728159B2uspto-grants-2010_06