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12th December 2012 @ 02:51
Synthesis of 1-ethoxy-1-oxopropan-2-yl 1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-carboxylate through formation of ester bond between 1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-carboxylic acid and ethyl 2-bromopropanoate.

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Reaction start time: 12:00 PM EST 5/12/12
MRN 57-1 (0.97 g,) was dissolved in DMF (10 mL), then Potassium Carbonate (1.5 g) was added after. The mixture was stirred at room temperature for 30 minutes, followed by addition of Ethyl-2-bromopropionate (0.8 mL, ) and was left stirring at room temperature.

At 8:00 PM ethyl acetate:water (40 mL, 1:1) mixture was added to the reaction and extracted with ethyl acetate (3 × 20 mL) the organic layers were combined, washed with water (20 mL), then dried over magnesium sulfate and concentrated to a brown oil, which was left to dry overnight.

At 11:20 AM small pale yellow crystals had formed with some leftover brown oil. The mixture was dried under high vac for 1 hour. Remaining brown oil was decanted out and the crystals washed with hexane (10 mL) to give pale yellow crystals (0.52 g,)

Risk and Hazard assessment:
Same as Upscaled synthesis of 1-ethoxy-1-oxopropan-2-yl 1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-carboxylate (MD 17-2).
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