反应详情

To a slurry of 44.3 g 1-(4-chlorophenyl)-2-(1H-1,2,4-triazol-1-yl) ethanone in 800 ml dry toluene and 400 ml 1-butanol was added 31.2 g 2-mercaptoethanol and 51.0 g p-toluenesulfonic acid. The mixture was refluxed under a Dean-Stark trap for 48 hours. On cooling, a white solid precipitated out, which was removed by filtration. The filtrate was evaporated, the residue dissolved in dichloromethane and washed twice with 10% aqueous sodium hydroxide and once with water. The organic layer was dried, filtered and evaporated to leave an oil which was taken up in cyclohexane. The cyclohexane was evaporated to azeotrope off any remaining 1-butanol, leaving an oily solid which was triturated with petroleum ether to give 15.7 g of product.

1. temperatureThe mixture was refluxed under a Dean-Stark trap for 48 hours
2. temperatureOn cooling
3. customa white solid precipitated out
4. customwhich was removed by filtration
5. customThe filtrate was evaporated
6. dissolutionthe residue dissolved in dichloromethane
7. washwashed twice with 10% aqueous sodium hydroxide and once with water
8. customThe organic layer was dried
9. filtrationfiltered
10. customevaporated
11. customto leave an oil which
12. customThe cyclohexane was evaporated
13. customleaving an oily solid which
14. customwas triturated with petroleum ether