in tetrahydrofuran standing of the reaction mixture for 18 h at room temp.;; after removement of the solvent, extraction with CH2Cl2 and chromy.; recrystn. from petroleum ether/ ether and sublimation at 120°C/ 0.3 torr;;
参考文献
Blackmore, T.; Bruce, M. I.; Stone, F. G. A.
J. Chem. Soc. (London) A, 1968 , p. 2158 - 2162
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Gmelin Handbook: Ru: SVol., 202, page 541 - 544
in neat (no solvent) C6F4(CN)2 (2.4 mmol) and Zn(CH3COO)2 (0.6 mmol) mixed, three times flushed with N2 and vac., sealed in glass ampoule under vac., heated for 1 h at 180-190°C; S. Hiller, D. Schlettwein, N. R. Armstrong, D. Woehrle, J. Mater. Chem. 8, 945 (1998); washed with acetone and with petrol ether, treated in Soxhlet apparatus with H2O, then with petrol ether, dried, purified by sublimation in vac.at 350°C;
参考文献
Brinkmann; Kelting; Makarov; Tsaryova; Schnurpfeil; Woehrle; Schlettwein
Physica Status Solidi (A) Applications and Materials Science, 2008 , vol. 205, # 3 p. 409 - 420
in N,N-dimethyl-formamide other Radiation; to mixt. Zn(OAc)2*2H2O and phthalonitrile DMF was added and heated in microwave Discover CEM reactor to 200°C for 10 min in sealed tube; Soxhlet extraction with acetone, CH2Cl2, and MeCN followed by recrystn. from pyridine;
in further solvent(s) N2-atmosphere, 25percent stoich. excess of tetrafluorophthalonitrile, refluxing in 1-chloronaphtalene (24 h); cooling to room temp., filtration, addn. of petroleum ether, cooling in ice bath (pptn.), filtration, recrystn. (H2SO4);
参考文献
Balkus, Kenneth J.; Gabrielov, Alexei G.; Bell, Stephen L.; Bedioui, Fethi; Roue, Lionel; Devynck, Jacques
Inorganic Chemistry, 1994 , vol. 33, p. 67 - 72
