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18th February 2013 @ 05:56
Chlorination of sodium 1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-sulfonate using Phosphorous pentachloride.Reaction start time: 5:00 PM EST 18/2/13MD 6-5 (100 mg, 0.34 mmol, 1 equiv) and Phosphorous Pentachloride (72 mg, 0.34 mmol, 1 equiv) were mixed at room temperature in dry diethyl ether (5 mL) for 2 hours under an inert atmosphere. After 2 hours the mixture was filtered and to the filtrate was added pyridine (44 µL, 0.68 mmol, 2 equiv.) followed by N-methylbenzylamine (70 µL, 0.68 mmol, 2 equiv.), after addition a cloudy yellow percipitate formed. Removal of solvent under reduced atmosphere left behind a thick yellow oil (36 mg). See also:[blog=5642]Chlorination of sodium 1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-sulfonate (MD 15-1)[/blog], [blog=6586]Synthesis of sodium 1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-sulfonate (MD 6-5)[/blog]Risk and Hazard assessment: Same as[blog=5642] [/blog]