反应详情

2,2,6,6-Tetramethylbenzo[1,2-d:4,5-d']bis(1,3)dithiole (2.86 g, 10 mmol; prepared according to WO-91/12024) was dissolved in anhydrous THF (75 mL) and cooled to -70° C. n-Butyllithium (4.4 mL, 2.5M in hexane) was added. The reaction mixture was allowed to reach ambient temperature. 4-Methoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis-(1,3)-dioxole (1.4 g, 5 mmol) was added as a solid. After 1 hour, the mixture was quenched with saturated aqueous NaH2PO4. The aqueous phase was discarded and the organic layer evaporated. The residue was dissolved in dichloromethane, washed with water and dried (Na2SO4). The product was purified by column chromatography (dichloromethane:heptane, 1:1) giving 1.8 g (44%) of pure product.

1. customprepared
2. additionwas added
3. customto reach ambient temperature
4. customthe mixture was quenched with saturated aqueous NaH2PO4
5. customthe organic layer evaporated
6. dissolutionThe residue was dissolved in dichloromethane
7. washwashed with water
8. dry with materialdried (Na2SO4)
9. customThe product was purified by column chromatography (dichloromethane:heptane, 1:1)