反应详情

5.4 g of 3,3-dimethyl-5-hydroxy-2,3-dihydrobenzofuran was dissolved in 30 ml of tetrahydrofuran, and then 4.6 ml of triethylamine was added while stirring the solution. Then, 5.0 g of 3-chlorosulfonyl-1,2,4-triazole was gradually added while cooling with ice and stirring the solution. Then, this was stirred for 14 hours. Tetrahydrofuran was evaporated, and 2N hydrochloric acid was added and extracted with ethyl acetate. The organic layer was washed with brine, dried with magnesium sulfate, and the solvent was removed, so that coarse crystals were obtained. This was then recrystallized from n-hexane/ethyl acetate, so that 2.7 g of the titled compound was obtained.

1. temperaturewhile cooling with ice
2. stirringstirring the solution
3. stirringThen, this was stirred for 14 hours
4. customTetrahydrofuran was evaporated
5. addition2N hydrochloric acid was added
6. extractionextracted with ethyl acetate
7. washThe organic layer was washed with brine
8. dry with materialdried with magnesium sulfate
9. customthe solvent was removed
10. customso that coarse crystals were obtained
11. customThis was then recrystallized from n-hexane/ethyl acetate, so that 2.7 g of the titled compound
12. customwas obtained