反应详情

温度

0 °C

2,2,6,6-Tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxole (5.15 g, 23.2 mmol) was dissolved in dry ether (40.0 mL) in a dried, argon filled reaction vessel. The solution was cooled to 0° C. and n-butyllithium (9.29 mL, 2.5M in hexane) was added. After stirring for 15 min at ambient temperature, the mixture was cooled to 0° C. and 4-methoxycarbonyl-(2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dithiole) (4.0 g, 11.6 mmol) was added portionwise. The reaction was stirred at ambient temperature overnight. The voluminous precipitate was dissolved by addition of water (70 mL) and ether (50 mL). The organic layer was separated and the aqueous phase was washed once more with ether. The organic phase was dried (Na2SO4) and evaporated to give a semisolid residue. The product was recrystallized from acetonitrile. Yield of pure product was 5.26 g (60%).

1. additionfilled
2. customreaction vessel
3. temperaturethe mixture was cooled to 0° C.
4. stirringThe reaction was stirred at ambient temperature overnight
5. customThe organic layer was separated
6. washthe aqueous phase was washed once more with ether
7. dry with materialThe organic phase was dried (Na2SO4)
8. customevaporated
9. customto give a semisolid residue
10. customThe product was recrystallized from acetonitrile