HRID2379662

反应详情

EQUATION

反应方程式

HRID 2379662 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Separately, 3.12 g of 5-n-decyl-2-(4-hydroxyphenyl)pyrimidine and 0.53 g of potassium hydroxide were added to 14 ml of dimethylformamide, and the mixture was stirred for 3 hours at 100° C. To the mixture was added the above-prepared 2.98 g of 6-pentyloxyheptyl-p-toluenesulfonate followed by 5 hours of stirring under heating at 100° C. After the reaction, the reaction mixture was poured into 200 ml of cold water and acidified to about pH 3 with 6N-hydrochloric acid and extracted with benzene, followed by washing with water, drying with anhydrous magnesium sulfate and distilling-off of the solvent, to obtain 4.71 g of crude product. The product was purified by silica gel column chromatography (n-hexane/ethyl acetate=10/2) and recrystallized from hexane to obtain 1.56 g of 5-n-decyl-2-[4-(6-pentyloxyheptyloxy)phenyl]pyrimidine.

WORKUP

后处理

  1. waitfollowed by 5 hours
  2. stirringof stirring
  3. temperatureunder heating at 100° C
  4. customAfter the reaction
  5. extractionextracted with benzene
  6. washby washing with water
  7. dry with materialdrying with anhydrous magnesium sulfate and distilling-off of the solvent
  8. customto obtain 4.71 g of crude product
  9. customThe product was purified by silica gel column chromatography (n-hexane/ethyl acetate=10/2)
  10. customrecrystallized from hexane