HRID1414172

反应详情

EQUATION

反应方程式

HRID 1414172 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

68 g (0.5 mole of p-toluic acid were heated with 54.5 g (0.5 mole) of p-aminophenol and 2 g of boric acid in 750 ml of 1,2-methylnaphthalene and the water that formed was eliminated slowly by azeotropic destillation. After heating for 6 hours, 1 g of boric acid were added. After 12 hours, 16 ml of H2O (98%) passed over. The solvent was then removed until dryness, the residue was dissolved in 750 ml of ethanol, clarified with silica gel while still hot, and combined after filtration, while still hot, with 500 ml of H2O. After cooling and filtration with suction at room temperature and washing with aqueous ethanol, there were obtained 89.4 g (85.6% of the theory) of 2-p-tolyl-benzoxazole melting at 113° to 114° C. ##STR41##

WORKUP

后处理

  1. temperatureAfter heating for 6 hours
  2. customThe solvent was then removed until dryness
  3. dissolutionthe residue was dissolved in 750 ml of ethanol
  4. filtrationafter filtration
  5. temperatureAfter cooling
  6. filtrationfiltration with suction at room temperature
  7. washwashing with aqueous ethanol