FIELD: manufacturing technology.
SUBSTANCE: invention relates to methods of purifying substances from related hardly-separable impurities by crystallization, specifically to a method of purifying glycoluril (2,4,6,8-tetraazabicyclo[3.3.0]octane-3,7-dione) from hard-separable impurities of hydantoin (2,4-imidazolidinedione), wherein hydantoin is formed as a by-product (product of condensation of urea and glyoxal at high temperature in acidic medium) and content thereof should not exceed 0.1 %. Method of purifying glycoluril from admixture of hydantoin to hydantoin level of less than 0.1 % involves applying a crystallization method by successively dissolving glycoluril with a hydantoin admixture in 85 % orthophosphoric acid while heating to 60 °C, cooling the obtained solution to room temperature and adding acetonitrile in ratio, pts. wt.: glycoluril with a hydantoin impurity of 1, 85 % orthophosphoric acid 5, acetonitrile 4, followed by washing the residue with acetonitrile, filtering and drying.
EFFECT: disclosed is a method of purifying glycoluril from hydantoin impurities.
1 cl, 1 dwg
Title | Year | Author | Number |
---|---|---|---|
METHOD OF PRODUCING 2,4,6,8-TETRAAZBICYCLO[3,3,0]OCTANE-3,7-DIONE | 2010 |
|
RU2439072C1 |
METHOD OF OBTAINING GLYCOURIL | 2014 |
|
RU2583110C1 |
METHOD FOR PRODUCTION OF 2,4,6,8- TETRACETYL -2,4,6,8- TETRAZABICYCLO[3,3,0]OCTANE- 3,7-DION | 1991 |
|
RU2050358C1 |
METHOD OF SYNTHESIS OF 2,6-DIACETYL-1,5-DI-(R)-2,4,6,8-TETRAAZABICYCLO[3,3,0]OCTANE- 3,7-DIONES | 1991 |
|
RU2021272C1 |
METHOD OF SYNTHESIS OF 2,6-DISUBSTITUTED 2,4,6,8-TETRAAZABICYCLO[3,3,0]OCTANE-3,7-DIONES | 1990 |
|
RU2021273C1 |
METHOD FOR GLYOCARB OLIGOMER PREPARATION | 2015 |
|
RU2612257C1 |
METHOD FOR ISOLATING SPATIAL ISOMERS OF N, N'-DIMETHYLGLYCOLURIL | 2017 |
|
RU2665714C1 |
METHOD OF SYNTHESIS OF AROMATIC 1,2-DIKETONES | 1990 |
|
RU2024484C1 |
METHOD OF FOOTING GLUEING TO SHOE UPPER PART | 1993 |
|
RU2079533C1 |
VOLTA-PARAMETRIC METHOD OF DETERMINATION OF TOTAL CHOLESTEROL IN BIOLOGICAL OBJECTS | 2016 |
|
RU2629836C1 |
Authors
Dates
2019-12-09—Published
2019-10-11—Filed