反应详情

2-Thiazolecarboxaldehyde (1 g) was dissolved in toluene (50 ml), followed by the addition of trimethylene glycol (3.36 g) and p-toluenesulfonic acid (17 mg). The resulting mixture was heated under reflux with a Dean-Stark apparatus for 4 hr. After cooling as it was, the reaction mixture was washed sequentially with an aqueous solution of saturated sodium bicarbonate and brine, dried (over MgSO4) and evaporated. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane system), to give the title compound as a brown solid (1.104 g, yield; 73%).

1. temperatureThe resulting mixture was heated
2. temperatureunder reflux with a Dean-Stark apparatus for 4 hr
3. temperatureAfter cooling as it
4. washthe reaction mixture was washed sequentially with an aqueous solution of saturated sodium bicarbonate and brine
5. dry with materialdried (over MgSO4)
6. customevaporated
7. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane system)