HRID1076877

反应详情

EQUATION

反应方程式

HRID 1076877 的结构方程式

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a mixture of 1.6 g. of 2-methoxynaphthalene, 1.6 g. of acetyl chloride, and 20 ml. of nitrobenzene, there are added 4.0 g. of aluminum chloride. The resulting mixture is stirred for 48 hours at 25°C; then it is washed with water until free of chloride ion. The mixture is dried over sodium sulfate and evaporated under reduced pressure. The residue, 2-acetyl-6-methoxynaphthalene, is refluxed in 2 ml. of morpholine containing one-half gram of sulfur for 2 hours; the reaction mixture is then filtered and evaporated. The resulting reaction derivative is extracted with diethyl ether; the extracts are combined and evaporated. The residue is refluxed in 10 ml. of concentrated hydrochloric acid for 2 hours, cooled to 25°C, and neutralized with aqueous sodium hydroxide. The mixture is then extracted with ether and the extracts are combined, washed with water to neutrality, dried and evaporated to yield 2-(6-methoxy-2-naphthyl)acetic acid.

WORKUP

后处理

  1. additionTo a mixture of 1.6 g
  2. washthen it is washed with water until free of chloride ion
  3. dry with materialThe mixture is dried over sodium sulfate
  4. customevaporated under reduced pressure
  5. temperatureThe residue, 2-acetyl-6-methoxynaphthalene, is refluxed in 2 ml
  6. waitof morpholine containing one-half gram of sulfur for 2 hours
  7. filtrationthe reaction mixture is then filtered
  8. customevaporated
  9. customThe resulting reaction derivative
  10. extractionis extracted with diethyl ether
  11. customevaporated
  12. temperatureThe residue is refluxed in 10 ml
  13. waitof concentrated hydrochloric acid for 2 hours
  14. temperaturecooled to 25°C
  15. extractionThe mixture is then extracted with ether
  16. washwashed with water to neutrality
  17. customdried
  18. customevaporated