反应详情

To 10 ml of tetrahydrofuran were dissolved 0.25 g (1.5 mmol) of 6,6-difluoro-5-methyl-5-hexene-1-thiol and 0.39 g (2.0 mmol) of benzo[b]thiophene-2-carbonylchloride, followed by the drop-wise addition of 0.30 g (3.0 mmol) of triethylamine at room temperature, followed by stirring at the same temperature for 1 hour. The reaction liquid was then poured in water and extracted with diethyl ether. The organic layer was washed with water and a saturated saline solution in this order, followed by drying over anhydrous magnesium sulfate and concentration under reduced pressure. The residue was purified with silica gel column chromatography (diisopropyl ether:hexane=1:20) to obtain 0.39 g (yield: 80%) of S-(6,6-difluoro-5-methyl-5-hexenyl) benzo[b]thiophene-2-thiocarboxylate.

1. customThe reaction liquid
2. extractionextracted with diethyl ether
3. washThe organic layer was washed with water
4. dry with materialby drying over anhydrous magnesium sulfate and concentration under reduced pressure
5. customThe residue was purified with silica gel column chromatography (diisopropyl ether:hexane=1:20)