HRID1587267

反应详情

EQUATION

反应方程式

HRID 1587267 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

0.34 g (1.0 mM) of 2-(4-hexylphenyl)-5-(4-hydroxyphenyl)-1,3-thiazole, 0.07 g of 85%-KOH and 12 ml of n-butanol were mixed. To the mixture, 0.29 g (1.0 mM) of 3-(trimethylsilyl)propyl p-toluenesulfonate was added dropwise under stirring at 100° C., followed by further stirring for 9 hours at 100° C. After the reaction, the reaction mixture was poured into water and extracted with ethyl acetate, followed by washing with water and drying with anhydrous magnesium sulfate. The magnesium sulfate in the resultant mixture was filtered off and the filtrate was condensed into a solid, followed by purification by silica gel column chromatography (eluent: toluene) and recrystallization from a mixture solvent (ethanol/ethyl acetate) to obtain 0.32 g of 2-(4-hexylphenyl)-5-[4-(3-trimethylsilylpropoxy)phenyl]-1,3-thiazole (Yield: 70.8%). ##STR81##

WORKUP

后处理

  1. stirringby further stirring for 9 hours at 100° C
  2. customAfter the reaction
  3. extractionextracted with ethyl acetate
  4. washby washing with water
  5. dry with materialdrying with anhydrous magnesium sulfate
  6. filtrationThe magnesium sulfate in the resultant mixture was filtered off
  7. customcondensed into a solid
  8. customfollowed by purification by silica gel column chromatography (eluent: toluene) and recrystallization from a mixture solvent (ethanol/ethyl acetate)