HRID441757

反应详情

EQUATION

反应方程式

HRID 441757 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

15 g of 4,4'-dimethyldiphenyl ether, 0.034 g (0.15 m. mole) of palladium acetate and 0.015 g (0.15 m. mole) of acetylacetone were placed in a glass vessel and this is placed in a 100 ml-autoclave. Then a mixture gas of nitrogen and oxygen of molar ratio 1:1 was filled in it to 50 kg/cm2 of inner pressure. The autoclave was shaken at 150° C. for 5 hours. After completion of the reaction, the reaction mixture was subjected to fractional distillation. After distilling out the unreacted 4,4'-dimethyldiphenyl ether, a distillate having b.p. 130°-135° C./12 mmHg was recrystallized from ethanol to give 2.6 g (13 m. moles) of 2,8-dimethyldibenzofuran. The obtained 2,8-dimethylbenzofuran showed m.p. 62°-64° C. (reference value, 64° C.).

WORKUP

后处理

  1. customAfter completion of the reaction
  2. distillationthe reaction mixture was subjected to fractional distillation
  3. distillationAfter distilling out the unreacted 4,4'-dimethyldiphenyl ether
  4. customwas recrystallized from ethanol