反应详情

温度

50 °C

Phosphorus oxychloride ("POCl3 ") (1 ml) was added into dimethyl formamide (20 ml) slowly under nitrogen gas atmosphere in ice bath and stirred for 1 hour. The dimethyl formamide solution (5 ml) of 5-hydroxymethyl-2,2'-bithiophene (0.5 g) was dropped in slowly. The mixture was stirred for half an hour at room temperature, then the temperature was raised to 50° C. and was further stirred for 3 hours. The reaction solution was poured into potassium carbonate ice water solution. Then the solution was extracted with 100 ml of ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residual solid was purified by column chromatography, eluted with ethyl acetate/n-hexane (3/7). Light yellowish product was recrystallized from ethyl acetate/n-hexane mixture. The melting point of the product was 123°-124° C. The yield was 85%.

1. stirringThe mixture was stirred for half an hour at room temperature
2. stirringwas further stirred for 3 hours
3. extractionThen the solution was extracted with 100 ml of ethyl acetate
4. washThe extract was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was removed under reduced pressure
7. customthe residual solid was purified by column chromatography
8. washeluted with ethyl acetate/n-hexane (3/7)
9. customLight yellowish product was recrystallized from ethyl acetate/n-hexane mixture
10. customwas 123°-124° C