HRID1384412

反应详情

EQUATION

反应方程式

HRID 1384412 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 17.62 g of 2-hydroxy-4′-methoxyacetophenone (Kovach et al., J. Amer. Chem. Soc., Vol. 115, No. 23, (1993) p. 10476) and 12.96 g of pyridine in 240 ml of dichloromethane, a solution of 26.32 g of eugenol-chloroformate in 60 ml of dichloromethane was dropped in at 5-10° C. Then, the mixture was stirred for 6 hours at room temperature. The reaction mixture was then acidified with 2N HCl and extracted with ether. The combined organic phases were washed with 2N HCl, saturated sodium bicarbonate and brine, and then dried, filtered, and evaporated to dryness. The resulting solid was purified by recrystallization to yield 29.79 g of yellow crystals.

WORKUP

后处理

  1. extractionextracted with ether
  2. washThe combined organic phases were washed with 2N HCl, saturated sodium bicarbonate and brine
  3. customdried
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customThe resulting solid was purified by recrystallization