反应详情

To 5 ml of 2-chlorotoluene was dissolved 0.20 g (0.64 mmol) of 6,6-difluoro-5-methyl-5-hexenyl benzo[b]thiophene-2-carboxylate, followed by the addition of 0.26 g (0.64 mmol) of Lawesson's reagent and stirring by heating under refluxing for 4 hours. To the reaction liquid were added 2 ml of isopropyl ether and 10 ml of hexane and precipitated solid was filtered off. The filtrate was concentrated under reduced pressure and the residue was purified with silica gel column chromatography (diisopropyl ether:hexane=1:30) to obtain 0.17 g (yield: 81%) of O-(6,6-difluoro-5-methyl-5-hexenyl) benzo[b]thiophene-2-thiocarboxylate.

1. temperatureby heating
2. temperatureunder refluxing for 4 hours
3. customTo the reaction liquid
4. customprecipitated solid
5. filtrationwas filtered off
6. concentrationThe filtrate was concentrated under reduced pressure
7. customthe residue was purified with silica gel column chromatography (diisopropyl ether:hexane=1:30)