FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5,5,0,03.11,05.9] dodecane, including catalytic hydrogenation of 4,10-dibenzyl-2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5,5,0,03.11,05.9]dodecane using a spent catalyst, hydrogen supply under pressure, wherein hydrogenation of 4,10-dibenzyl-2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5,5,0,03.11,05.9]dodecane is carried out in a mixed with a catalyst, spent at step of catalytic hydrogenation of 2,4,6,8,10,12-hexabenzyl-2,4,6,8,10,12-hexaazatetracyclo[5,5,0,03.11,05.9]dodecane, for 10–40 minutes, wherein ratio of 4,10-dibenzyl-2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo[5,5,0,03.11,05.9]dodecane to spent catalyst is 3.0–5.0, and feeding of hydrogen during hydrogenation is carried out when reaction mass reaches temperature of 85–99 °C.
EFFECT: method of producing 2,6,8,12-tetraacetyl-2,4,6,8,10,12-hexaazatetracyclo [5,5,0,03,11,05,9] dodecane, which enables to simplify process, reducing duration thereof with simultaneous increase of output and purity of end product due to optimisation of characteristics of used reagents and conditions of introduction into process.
1 cl, 2 ex
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Authors
Dates
2017-02-14—Published
2015-07-23—Filed