HRID1587269

反应详情

EQUATION

反应方程式

HRID 1587269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2 ml of toluene was added to 0.81 g (1.99 mM) of 2-(4-hexylphenyl)-5-(4-allylcarbonyloxyphenyl)-1,3-thiazole, followed by stirring at room temperature. To the mixture, an appropriate amount chloroplatinic acid, three drops of isopropyl alcohol and 0.24 g (2.06 mM) of butyldimethylsilane were successively added and heated to 80° C., followed by stirring for 7 hours. After the reaction, the reaction mixture was poured into water, followed by extraction with ethyl acetate. The organic layer was washed with water and dried with anhydrous magnesium sulfate. The magnesium sulfate in the resultant organic layer was filtered off, followed by distilling-off of the solvent, purification by silica gel column chromatography (eluent: toluene) and recrystallization from a mixture solvent (methanol/toluene) to obtain 0.25 g of 2-(4-hexylphenyl)-5-[4-(3-butyldimethylsilylpropylcarbonyloxy)phenyl]-1,3-thiazole (Yield: 24.3%). ##STR83##

WORKUP

后处理

  1. temperatureheated to 80° C.
  2. stirringby stirring for 7 hours
  3. customAfter the reaction
  4. extractionfollowed by extraction with ethyl acetate
  5. washThe organic layer was washed with water
  6. dry with materialdried with anhydrous magnesium sulfate
  7. filtrationThe magnesium sulfate in the resultant organic layer was filtered off
  8. distillationfollowed by distilling-off of the solvent, purification by silica gel column chromatography (eluent: toluene) and recrystallization from a mixture solvent (methanol/toluene)