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11th December 2012 @ 23:35
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Ethyl acetoacetate (19.4 mL, 15.4 mmol, 1 equiv) was diluted in water (20 mL) and cooled to 0 ˚C with stirring. Aqueous ammonia (28%, 15.4 mL, 18.5 mmol, 1.2 equiv.) was added and the reaction mixture stirred for 5 mins at 0 ˚C, prior to the dropwise addition of chloroacetone (12.8 mL, 15.4 mmol, 1 equiv.) and the pale yellow solution stirred at 0 ˚C. The reaction mixture was stirred for 3 hours at rt and the white precipitate formed was filtered and washed with water to provide the desired product, 6.7 g. The filtrate (a red solution) was then left to stir at rt overnight and the resulting precipitate filtered and washed to give a red sludge containing a few crystals. The sludge was washed into the aqueous layers with DCM and then extracted (DCM x 3). Separating funnel broke and product lost to fumehood floor. Very unpleasant smelling compound so the mess was cleared up and no attempt was made to recover the product.