CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE; INSTITUT NATIONAL DE LA SANTE ET DE LA RECHERCHE M; RHODIA UK LIMITED
Patent: US2009/142316 A1, 2009 ;
Location in patent: Page/Page column 156 ;
in tetrahydrofuran 9 h; Heating; Yield given. Further byproducts given. Yields of byproduct given. Title compound not separated from byproducts;
参考文献
Mitropol'skaya, G. I.; Kireev, V. V.; Korshak, V. V.; Goryaev, A. A.
J. Gen. Chem. USSR (Engl. Transl.), 1982 , vol. 52, # 11 p. 2486 - 2491,2197 - 2201
in neat (no solvent) condensation of 80 ml liquid SO2 on a mixt. of 200 g (NPCl2)3 and 300 g KF; heating at 98-100 °C for 22 days;; removal of an excess of SO2; fractionation, transition temp. 49-49.8 °C at 747 Torr; yield 115.3 (NPCl2)3;;
参考文献
Chapman, A. C.; Paddock, N. L.; Paine, D. H.; Searle, H. T.; Smith, D. R.
Journal of the Chemical Society, 1960 , p. 3608 - 3614
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Gmelin Handbook: P: MVol.C, 238, page 544 - 546
H2O or HF in nitrobenzene dissolving (NPCl2)3 in freshly distd. C6H5NO2; addn. of an excess of NaF or a small amount of H2O or HF under exclusion of H2O (drying tube with P2O5); heating on refluxing;; fractionation;;
