HRID1395682

反应详情

EQUATION

反应方程式

HRID 1395682 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

12.2 g of acetyl chloride was added to a mixture of 10.3 g of 1B, and 120 ml of carbon disulfide, then 21.8 g of anhydrous aluminum chloride was added in portions to the stirred mixture. The mixture then was stirred at room temperature for 2.5 hours, the temperature rising to 32° C. The mixture was poured into 1 liter of ice water, the mixture was stirred for 30 minutes, and the solution was extracted with ether. The extract was dried (MgSO4) and concentrated. The residue was washed with ether and dried. It was dissolved in 100 ml of chloroform, the solution was treated with a decolorizing agent, and 100 ml of hexane was added. The resulting solution was concentrated to about 100 ml and cooled to give ethyl 5-(4-acetylphenyl)benzofuran-2-carboxylate (6A), mp: 105°-107° C.

WORKUP

后处理

  1. customrising to 32° C
  2. stirringthe mixture was stirred for 30 minutes
  3. extractionthe solution was extracted with ether
  4. dry with materialThe extract was dried (MgSO4)
  5. concentrationconcentrated
  6. washThe residue was washed with ether
  7. customdried
  8. dissolutionIt was dissolved in 100 ml of chloroform
  9. additionthe solution was treated with a decolorizing agent, and 100 ml of hexane
  10. additionwas added
  11. concentrationThe resulting solution was concentrated to about 100 ml
  12. temperaturecooled