反应详情

温度

0 °C

A solution (0.25 M) of methyl 6-cyclohexyl-5-phenyl-4H-thieno[3,2-b]pyrrole-2-carboxylate in DMF at 0° C. was treated with NaH (1.5 eq., 60% dispersion in mineral oil), and the suspension was stirred at 0° C. for 60 min then it was treated with chloromethyl methyl ether (5 eq.). The mixture was stirred at RT for 2 h then it was quenched with ice/water and extracted with AcOEt. The combined organic phase was washed with brine and dried. Evaporation of the solvent under reduced pressure gave a residue that was purified by flash chromatography on silica gel (1:12 acetone/toluene) to afford the title compound (92%) as an oil.

1. stirringThe mixture was stirred at RT for 2 h
2. customit was quenched with ice/water
3. extractionextracted with AcOEt
4. washThe combined organic phase was washed with brine
5. customdried
6. customEvaporation of the solvent under reduced pressure
7. customgave a residue that
8. customwas purified by flash chromatography on silica gel (1:12 acetone/toluene)