Process for the preparation of monomeric tetramethoxymethylglycoloril

In a process for the preparation of tetramethoxymethylglycoluril of the type having the sequential steps of (I) methylolating glycoluril with formaldehyde, (II) etherifying with methanol in a volatile solvent, and (III) isolating the tetramethoxymethylglycoluril product, the improvement comprising adding between steps (II) and (III) the sequential steps of:

• (IIa) separating the volatiles by distilling at a pH in the range of from about 5.0 to less than 7, at a temperature, pressure, and for a length of time sufficient to produce substantially fully methylolated, partially etherified, substantially monomeric tetramethoxymethylglycoluril, and
• (IIb) etherifying further the partially etherified tetramethoxymethylglycouril of step (IIa) with added methanol under acidic conditions to produce a substantially fully methylolated, substantially fully etherified, substantially monomeric tetramethoxymethylglycouril having a monomeric tetramethoxymethylglycoluril content in the range of from about 80 weight percent to 100 weight percent, a methoxy to methylene ratio in the range from about 0.95 to about 1.00, and a methylene to glycoluril ratio in the range of from about 3.7 to about 4.00.