反应详情

2.33 g of 2.4-dichloro-3-methylphenol was dissolved in 15 ml of tetrahydrofuran, and 1.84 ml of triethylamine was added while stirring the solution. Then, 2.0 g of 3-chlorosulfonyl-1,2,4-triazole was gradually added while cooling with ice and stirring the solution. Then, the solution was stirred at room temperature for 14 hours. Tetrahydrofuran was removed by distillation at reduced pressure, 2N hydrochloric acid was added, and extracted with ethyl acetate. The organic layer was washed with brine, and dried with magnesium sulfate. Then, the solvent was removed by distillation, so that coarse crystals were obtained. The coarse crystals were recrystallized from n-hexane/ethyl acetate, so that 2.25 g of the titled compound was obtained.

1. temperaturewhile cooling with ice
2. stirringstirring the solution
3. stirringThen, the solution was stirred at room temperature for 14 hours
4. customTetrahydrofuran was removed by distillation at reduced pressure, 2N hydrochloric acid
5. additionwas added
6. extractionextracted with ethyl acetate
7. washThe organic layer was washed with brine
8. dry with materialdried with magnesium sulfate
9. customThen, the solvent was removed by distillation
10. customso that coarse crystals were obtained
11. customThe coarse crystals were recrystallized from n-hexane/ethyl acetate, so that 2.25 g of the titled compound
12. customwas obtained