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With triethylamine In toluene Ambient temperature;
With sodium carbonate; triethylamine In dichloromethane
2 Preparation of N,N-dimethyl-N,N'-dibutyl-malonamide
Example 2 Preparation of N,N-dimethyl-N,N'-dibutyl-malonamide This amide is prepared by reacting commercial N-methyl-N-butyl amine with malonyl chloride in accordance with the following reaction diagram: STR8 To this end, one mole of N-methyl-N-butyl-amine and 1 mole of triethylamine are dissolved in 300 ml of methylene chloride. This is followed by cooling to 10° C. and progressively adding to the reaction medium 0.5 mole of malonyl chloride in 150 ml of methylene chloride. Addition takes place slowly because the reaction is highly exothermic. Following this addition, the reaction medium is allowed to return to ambient temperature, followed by stirring for two hours. Washing then takes place on a number of occasions with water in order to eliminate the hydrochloride, then once with 10% sodium carbonate solution in order to eliminate the residual acid and then on a further occasion with water. This is followed by drying and expulsion of the solvent, the sought product distilling at 140° to 144° C. under 0.3 mmHg, with a yield of 45%. The product is then recrystallized in hexane and in this way white crystals with a melting point of 52° C. are obtained. The product is characterized by potentiometric determination and by nuclear magnetic resonance of the proton in CDCl3, whilst using TMS as the reference. The NMR results obtained are given in the attached Table 2, and the potentiometric determination gives a purity of 99%.
Stage #1: N,N'-dimethyl-N,N'-dibutylmalonamide With sodium hydride In hexane; N,N-dimethyl-formamide; mineral oil at 0 - 20℃;
Stage #2: 1-(6-bromohexyl)-3-methylimidazolium bis(trifluoromethylsulfonyl)imide In hexane; N,N-dimethyl-formamide; mineral oil at 80℃; for 24h;
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