HRID1181673

反应详情

EQUATION

反应方程式

HRID 1181673 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

3-Iodo-2-methylpropane (4.6 g) and potassium carbonate (8.62 g) were added to a solution of 6-Chloro-3-methylpyrimidine-2,4[1H,3H]-dione (2.0 g) in dimethylformamide (10 ml). The mixture was heated at 90° C. for 18 hours then cooled to room temperature. The solution was diluted with 5% aqueous HCl solution until solution becomes acidic and extracted twice with diethyl ether. The combined organic extracts were dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure. The residue was purified by column chromatography over silica eluting with hexanes: ethyl acetate (1:1) to give the subtitle compound (1.5 g).

WORKUP

后处理

  1. temperaturethen cooled to room temperature
  2. extractionextracted twice with diethyl ether
  3. dry with materialThe combined organic extracts were dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue was purified by column chromatography over silica eluting with hexanes: ethyl acetate (1:1)