FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing O-luminolates of alkali metals. The method includes reacting 3-nitrophthalic acid with hydrazine hydrate to form 5-nitro-2,3-dihydro-1,4-phthalazinedione, reducing the nitro groups and obtaining alkali metal salts. The cyclisation reaction is carried out in a medium of concentrated acetic acid at boiling point. Reduction of the nitro groups with simultaneous formation of alkali metal salts is carried out in an aqueous alkaline medium using hydrogen as a reducing agent at pressure of 1-5 atm and temperature of 90-110°C and a Raney nickel catalyst. After crystallising, separating, washing and drying the crystals, associates of hydrate forms of O-metallated luminal having the following general formula are obtained: , M-Li, n=1; (VIIIa), M-Na, n=2; (VIIIb), M-K, n=3; (VIIIc), m=2.
EFFECT: invention enables to obtain associates of hydrate forms of O-metallated luminal using a method which improves stability of process parameters, minimises harmful impurities and provides an environmentally safe process.
7 dwg, 3 tbl, 3 ex
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Authors
Dates
2014-10-27—Published
2013-05-22—Filed