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Replace dimethyl sulfate
Hi,
SWIM has found this synth.-desc.:
Methyl methyl acetoacetate (3)
4440 grams of methyl acetate, containing 2% methyl alcohol, was weighed into a. 12L flask provided with a reflux condenser. 230g of sodium metal in the form of small pieces (~1 cm3) was added to the methyl acetate at once. Heat was applied to bring the reaction mixture to reflux. After 11h all of the sodium dissolved. Excess methyl acetate was then distilled from the reaction mixture until all of the methanol azeotrope distilled off. 5 L of toluene was then added and distillation continued until the last of the methyl acetate was recovered. 1200g of dimethyl sulfate was then added over a period of 2h at refluxing temperature. Refluxing was continued until reaction was neutral. The reaction mixture was then cooled to room temperature, and 1400 mL of water added to dissolve the sodium methyl sulfate. The oil layer was separated, washed with 2x1000 mL water and then fractionately distilled to give 882g methyl methyl acetoacetate (3), bp 76-76.5°C/20mmHg. 1700g of methyl acetate was recovered as constant boiling mixture, balance was recovered with the toluene.
What could replace the dimethyl sulfate, because its hardly to get in ger.
methyl iodide is much to expensive for SWIM
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