HRID13737

反应详情

EQUATION

反应方程式

HRID 13737 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

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.

WORKUP

后处理

  1. additionwas added
  2. filtrationthe catalyst was filtered off
  3. customThe organic layer was separated
  4. extractionthe aqueous phase was extracted with ether (2×50 ml)
  5. washThe combined organic extracts were washed with water (25 ml)
  6. dry with materialdried with anhydrous magnesium sulphate
  7. concentrationconcentrated