HRID327584

反应详情

EQUATION

反应方程式

HRID 327584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 8.0 g of anhydrous aluminum chloride and 3.59 of itaconic acid anhydride in dried tetrachloroethane was stirred for one hour at room temperature. To this solution, 4.39 g of 2-ethylbenzofuran dissolved in 10 ml of tetrachloroethane was added dropwise under cooling by ice-water. And then stirring was continued for 3 hrs. in ice-water and for 12 hrs. at room temperature. The reaction mixture was poured into the mixture of 80 g of ice and 20 ml of conc. HCl, then extracted with ethylacetate (50 ml). After washed with water, the solvent layer was made alkaline with 10% NaCO3 solution. The water layer was acidified with 10% HCl again and then extracted with ethylacetate. The brown viscous residue obtained after washing, drying and removal of ethyl acetate layer, was extracted with ligroin. After standing overnight, the needle-like crystals were obtained.

WORKUP

后处理

  1. additionwas added dropwise
  2. stirringAnd then stirring
  3. waitwas continued for 3 hrs
  4. customat room temperature
  5. extractionextracted with ethylacetate (50 ml)
  6. washAfter washed with water
  7. extractionextracted with ethylacetate
  8. customThe brown viscous residue obtained
  9. washafter washing
  10. customdrying
  11. customremoval of ethyl acetate layer
  12. extractionwas extracted with ligroin
  13. waitAfter standing overnight
  14. customthe needle-like crystals were obtained