HRID1285243

反应详情

EQUATION

反应方程式

HRID 1285243 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.67 g (13.6 mmole) of 1-bromo-5-[2-n-propyl-3-hydroxy-4-acetylphenoxy]-pentane, 2.39 g (8.65 mmole) of 2-carboethoxy-7-hydroxy-8-n-propylchromone, and 2.76 g (20 mmole) of anhydrous potassium carbonate were dissolved in 100 ml dimethylformamide in a 250 ml single neck round bottom flask equipped with a magnetic stirring bar and a drying tube charged with calcium chloride. The contents of the flask were stirred at 70° for 18 hours. After cooling, the reaction solution was filtered and the dimethylformamide removed by rotary evaporation. The residual dark red oil was dissolved in 50% ethyl acetate/hexane and purified by chromatography to give 2.07 g (44%) of the title compound, mp 90°-91°. Calc: C, 69.13; H, 7.11; Found: C, 69.44; H, 7.44.

WORKUP

后处理

  1. customequipped with a magnetic stirring bar and a drying tube
  2. temperatureAfter cooling
  3. filtrationthe reaction solution was filtered
  4. customthe dimethylformamide removed by rotary evaporation
  5. dissolutionThe residual dark red oil was dissolved in 50% ethyl acetate/hexane
  6. custompurified by chromatography