PURPOSE: To obtain the titled compound useful as a polar aprotic solvent efficiently in high selectivity and yield at a low cost, by reacting specific amounts of N-dimethylethylenediamine with urea in a polar solvent at temperature in two stages.
CONSTITUTION: N,N-Dimethyletylenediamine and urea in a molar amount of about twice based on the N,N-dimethylethylenediamine are charged into a polar solvent, e.g. 1,3-dimethyl-2-imidazolinone (abbreviated to DMI) having preferably ≥180°C boiling point and reacted at ≤140°C to give 1,1'-dimethyl-1,1'- dimethylenebisurea expressed by the formula which is the initial reaction product in almost the quantitative yield. The N,N-dimethylethylenediamine is then reacted and decomposed therewith at ≥180°C to give almost equimolar amounts of the N,N-dimethylethylenediamine and the urea to be used in the overall reaction while adding the N,N-dimethylethylenediamine to suppress the formationof cyanuric acid as a by-product and carry out the reaction in the latter stage. Thus, the aimed DMI is obtained. The overall reaction can be carried out under ordinary pressure.
JP2004115402 | METHOD FOR PRODUCING N,N'-DIALKYL CYCLIC UREA COMPOUND |
JPS5976065 | CARCINOSTATIC AGENT |
JPH11152272 | SEPARATION OF APROTIC POLAR SOLVENT BY LIQUID |
KAJIMOTO NOBUYUKI
WADA MASARU
MIZUTA HIDEKI