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4th November 2013 @ 09:37

pyrazine-2-carboxylic acid (12.5 g) was added to methanol (100 ml), and concentrated sulfuric acid(0.625 ml) was gradually added dropwise whilst stirring. The solution was refluxed at a temperature of 85oC for 22 hours, then cooled to room temperature and concentrated to a volume of 25 ml. Methylenechloride (50 ml) and water (25 ml) were added to the concentrate after which the solution was neutralised by gradual addition of saturated siodium bicarbonate (25 ml) to get a pH of approximately 8.5. An organic layer was seperated and a water layer was extracted again using methylenechloride (25 ml). The combined organic layer was dried over anhydrous magnesium sulfate, filtered , and washed with methylenechloride (5 ml). Methylenechloride was removed under vacumm to yield a yellow solid product (11.64 g) Melting point 60oC - 62oC. 1H NMR of solid product was derived (EO 4-1 1H NMR)

Attached Files
risk assesment EO 4-1.doc
Reaction Scheme EO 4-1.jpg
EO 4-1 1H NMR.pdf