HRID616423

反应详情

EQUATION

反应方程式

HRID 616423 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

An autoclave is charged with 18.1 g. o-nitrophenyl acetate, 2.50 g. 5% palladium-on-carbon, 0.50 g. ferric chloride 25 ml. acetic anhydride and 75 ml. acetic acid, purged with nitrogen, pressurized to 5,000 psig. with carbon monoxide, and heated at 190° C. for 5 hours. Analysis of the reaction mixture by vapor phase chromatography indicates complete conversion of the o-nitrophenyl acetate to 2-methylbenzoxazole. The catalyst is separated by filtration and washed with acetone. The solvents are evaporated and the residual oil is dissolved in ether and the solution is washed with aqueous sodium bicarbonate and water. After evaporation of the ether, the crude product is distilled to obtain 2-methylbenzoxazole, b.p.30 mm. 102°-110° C. The product is identical with an authentic sample of 2-methylbenzoxazole by vapor phase chromatography and infrared spectrum.

WORKUP

后处理

  1. additionAn autoclave is charged with 18.1 g
  2. customacetic acid, purged with nitrogen
  3. customThe catalyst is separated by filtration
  4. washwashed with acetone
  5. customThe solvents are evaporated
  6. dissolutionthe residual oil is dissolved in ether
  7. washthe solution is washed with aqueous sodium bicarbonate and water
  8. customAfter evaporation of the ether
  9. distillationthe crude product is distilled