HRID1791998

反应详情

EQUATION

反应方程式

HRID 1791998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 8-chloro-1,3-dimethyl-3,7-dihydropurine-2,6-dione (10.7 g), allyl bromide (5.2 ml), anhydrous potassium carbonate (10.3 g), and N,N-dimethylformamide (75 ml) was stirred at room temperature overnight. The reaction mixture was extracted with ethyl acetate and water, and the organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and filtered through a small amount of silica gel. The silica gel was washed with ethyl acetate, and the eluate was concentrated under reduced pressure. Recrystallization of the residue from ethyl acetate (50 ml) and hexane (100 ml) gave 10.57 g of the title compound.

WORKUP

后处理

  1. extractionThe reaction mixture was extracted with ethyl acetate and water
  2. washthe organic layer was washed with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered through a small amount of silica gel
  5. washThe silica gel was washed with ethyl acetate
  6. concentrationthe eluate was concentrated under reduced pressure
  7. customRecrystallization of the residue from ethyl acetate (50 ml) and hexane (100 ml)