反应详情

温度

200 °C

To a solution of 6-cyano-2-methyl-4H-thieno[3,2-b]pyrrole-5-carboxylic acid (0.54 g) in quinoline (10 mL) was added Copper powder (33 mg), and the mixture was stirred at 200° C. for 30 minutes using microwave reactor. To the reaction solution was added water, and a precipitated insoluble matter was filtered through a Celite pad (registered trademark). The organic layer was separated and the aqueous layer was extracted with ethyl acetate. The combined organic layer was washed with 1 mol/L hydrochloric acid, water and brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=76/24−53/47) to give the title compound (0.37 g).

1. filtrationa precipitated insoluble matter was filtered through a Celite pad (registered trademark)
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted with ethyl acetate
4. washThe combined organic layer was washed with 1 mol/L hydrochloric acid, water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe obtained residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=76/24−53/47)