HRID1939169

反应详情

EQUATION

反应方程式

HRID 1939169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 2,7-dichloroquinoxaline (2.8 g, 14.1 mmol), methyl 2-(4-hydroxyphenoxy)propanoate (2.76 g, 14.1 mmol), and pulverized potassium carbonate (3.9 g, 28.2 mmol) in acetone (70 mL) was refluxed for 3 hours. The reaction mixture was cooled to room temperature and methylene chloride and water were added to the reaction mixture. The organic phase was removed, and the aqueous phase was extracted with methylene chloride. The combined organic phase was washed with water, dried over potassium carbonate, concentrated, and dried under high vacuum. The product was purified by flash chromatography with 6:1 petroleum ether:ethyl ether to afford the desired product (2.8 g, 55% yield) as a solid: mp 103° C.; MS m/e 359 (M+ +H). Anal. Calcd for C18H15ClN2 O4 : C., 60.26; H, 4.21; N, 7.81; Cl, 9.88. Found: C, 60.44, H, 4.31; N, 7.69, Cl, 9.98.

WORKUP

后处理

  1. temperaturewas refluxed for 3 hours
  2. customThe organic phase was removed
  3. extractionthe aqueous phase was extracted with methylene chloride
  4. washThe combined organic phase was washed with water
  5. dry with materialdried over potassium carbonate
  6. concentrationconcentrated
  7. customdried under high vacuum
  8. customThe product was purified by flash chromatography with 6:1 petroleum ether