反应详情

Sodium carbonate (22.4 g, 0.21 mol), methyl iodide (30 g, 0.21 mol), and [2-(2-fluorobenzoyl)-1H-pyrrol-1-yl]-carbamic acid, ethyl ester (25.4 g, 0.09 mol) were combined in 100 ml of dry DMF with stirring at ambient temperature. After 72 hours, the mixture was poured into 800 ml of H2O and extracted with three 250 ml portions of DCM. The combined extracts were washed with H2O and brine, dried (MgSO4), filtered and evaporated to an oil. This oil was purified by HPLC (silica, DCM) to give 26 g (97%) of crystals, m.p. 64°-66°.

1. extractionextracted with three 250 ml portions of DCM
2. washThe combined extracts were washed with H2O and brine
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customevaporated to an oil
6. customThis oil was purified by HPLC (silica, DCM)