反应详情

温度

80 °C

A stirred solution of 4-methylbenzene-1,2-dithiol (0.5 g) in anhydrous DMF (50 ml) was treated with K2CO3 and 3,4-dichloro-1-methyl-pyrrole-2,5-dione (0.73 g) and stirred for about 7 hours at 80° C. The reaction mixture was poured into water and extracted with MTBE. The combined organic phases were washed once with water and after removal of the solvent under reduced pressure the crude product (0.85 g) was purified by flash column chromatography on silica gel (cyclohexane/ethyl acetate 9:1) to yield the compound ex. I-2 (0.25 g); m.p.: 171-176° C.

1. extractionextracted with MTBE
2. washThe combined organic phases were washed once with water
3. customafter removal of the solvent under reduced pressure the crude product (0.85 g)
4. customwas purified by flash column chromatography on silica gel (cyclohexane/ethyl acetate 9:1)
5. customto yield the compound ex