反应详情

A slurry of 1.8 g of [(2-cyclobutyl-4-thiazolyl)methyl] triphenylphosphonium chloride, in 80 ml of tetrahydrofuran was sealed under a positive argon atmosphere and the mixture cooled with an ice bath. Sodium hydride (0.2 g; 50% oil dispersion) was added and stirring and cooling continued for 30 min afterwhich 0.6 g of 3-nitrobenzaldehyde was added. The cooling bath was removed and the mixture was stirred at room temperature for 1 hr. The mixture was then filtered, condensed in vacuo and the residual materials taken up in 100 ml of methylene chloride. This solution was then washed with water, dried (MgSO4) and condensed in vacuo to yield 0.8 g of (E)-2-cyclobutyl-4-[2-(3-nitrophenyl)ethenyl]thiazole; m.p. 112°-115° C.

1. temperaturethe mixture cooled with an ice bath
2. temperaturecooling
3. additionwas added
4. customThe cooling bath was removed
5. stirringthe mixture was stirred at room temperature for 1 hr
6. filtrationThe mixture was then filtered
7. customcondensed in vacuo
8. washThis solution was then washed with water
9. customdried
10. custom(MgSO4) and condensed in vacuo