HRID2909

反应详情

EQUATION

反应方程式

HRID 2909 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

124.4 g (0.900 mol) potassium carbonate and 63 ml (0.547 mol) benzyl chloride were added in succession to a solution of 56.7 g (0.450 mol) 4-hydroxy-6-methyl-2H-pyran-2-one and 1.0 g (0.004 mol) 18-crown-6 in 900 ml anhydrous dimethyl-formamide. It was stirred vigorously for 4.5 hours at an internal temperature of 70°-75° C. It was suction filtered and the residue was washed well with ethyl acetate. The combined filtrates were extensively evaporated in a vacuum and subsequently poured onto ice water. The aspirated precipitate was recrystallized from t-butylmethyl ether after drying. 69.0 g (71%) V, melting point 92°-93° C.

WORKUP

后处理

  1. filtrationfiltered
  2. washthe residue was washed well with ethyl acetate
  3. customThe combined filtrates were extensively evaporated in a vacuum
  4. additionsubsequently poured onto ice water
  5. customThe aspirated precipitate was recrystallized from t-butylmethyl ether
  6. customafter drying