HCID 86720683, compound → HCID 71203605, compound

Participants

Reaction Conditions

Reaction Steps

Ethyl magnesium bromide (0.14 g, 1.1 ml, 1.06 mmol) was added drop wise to a solution of 5-(4′-(N-((dimethylamino)methylene)sulfamoyl)-6-methoxy-[1,1′-biphenyl]-3-yl)-N-methoxy-N,3,4-trimethylthiophene-2-carboxamide (Step 7, 0.11 g, 0.21 mmol) in anhydrous THF (10 ml) at 25° C. under stirring. The reaction mixture was then heated to 70-75° C. for 1 hour. The progress of the reaction was monitored by TLC. The reaction mixture was then cooled to 0° C. The cooled reaction mixture was then quenched with a saturated solution of ammonium chloride (10 ml). The resultant mixture was then extracted with ethyl acetate (3×20 ml). The combined organic layer was dried over anhydrous Na2SO4. The solvent was evaporated from the organic layer under reduced pressure to obtain a crude product, which was then purified by column chromatography using 35% ethyl acetate in hexane as an eluent to obtain the title compound 9 (0.03 g, 33.0%).

Provenance & Evidence