1,8-diazabicyclo[5.4.0]undec-7-ene in pentan-1-ol phthalonitrile (0.98 mmol) was treated with unsubstituted phthalonitrile(8.82 mmol) and Zn-contg. compd. (2.46 mmol) in pentanol at 140-150.deg ree.C for 24 h, then a small amt. of DBU was added; brief cooling; volatiles were removed under reduced pressure; residue was dissolved in CHCl3; soln. was filtered to remove ZnPc; filtrate was collected, evapd.to dryness in vac.; column chromy. (silica gel, CHCl3/CH3OH); recrystn. from THF/hexane; elem. anal.;
参考文献
Liu, Jian-Yong; Jiang, Xiong-Jie; Fong, Wing-Ping; Ng, Dennis K. P.
Organic and Biomolecular Chemistry, 2008 , vol. 6, # 24 p. 4560 - 4566
in water byproducts: CH3COOH; Irradiation (UV/VIS); 30percent H2O2 diluted with deionized water, Zn(CH3COO)2*2H2O dissolved in it;soln. irradiated by 35 W xenon lamp or sunlight for 6 h with continuous stirring; precursol sol aged for 2 days; baked at 40 °C overnight; dried;
in methanol; chloroform tetraphenylporphyrin (300 mg) and Zn(OAc)2*2H2O (800 mg) refluxed (1 h) in CHCl3/MeOH (2:1); cooled; solvent removed (vac.); dissolved in CHCl3; chromd. (silica, CHCl3);
参考文献
Vail, Sean A.; Schuster, David I.; Guldi, Dirk M.; Isosomppi, Marja; Tkachenko, Nikolai; Lemmetyinen, Helge; Palkar, Amit; Echegoyen, Luis; Chen, Xihua; Zhang, John Z. H.
Journal of Physical Chemistry B, 2006 , vol. 110, # 29 p. 14155 - 14166
in ethanol addn. of Zn-compound to hot soln. of ligand with stirring;; filtration of ppt.; washed (EtOH); dried (vacuum, 80°C);
参考文献
Baggio, Ricardo; Garland, Maria Teresa; Perec, Mireille
Journal of the Chemical Society, Dalton Transactions: Inorganic Chemistry (1972-1999), 1993 , # 22 p. 3367 - 3372
in ethanol High Pressure; Zn, Co salts in chosen atomic ratios added into EtOH; stirred vigorouslyfor 20 min at room temp.; soln. of NaOH in EtOH added; transferred into Teflon-lined stainless steel autoclave; sealed; heated to 120-250.degre e.C for 2 h; cooled to room temp.; ppt. collected; rinsed with H2O and abs. EtOH until pH about 7; dried inair at 60°C; identified by X-ray diffraction;
参考文献
Journal of Magnetism and Magnetic Materials, , vol. 321, # 19 p. 3352 - 3355
in ethanol
addn. of solid Zn(AcO)2*2H2O to ligand soln.; stirring at elevated temp. up to complete dissoln., 2h; cooling; pptn.; recrystn. (EtOH); elem. anal.;
参考文献
Dreher, Michael; Elias, Horst; Paulus, Helmut
Zeitschrift fuer Naturforschung, B: Chemical Sciences, 1987 , vol. 42, # 6 p. 707 - 710
in chloroform
stirring (reflux); removement of solvent (reduced pressure), chromy. (SiO2), recrystn. (heptane); elem. anal.;
参考文献
Sugiura, Ken-Ichi; Ponomarev, Gelii; Okubo, Satoshi; Tajiri, Akio; Sakata, Yoshiteru
Bulletin of the Chemical Society of Japan, 1997 , vol. 70, # 5 p. 1115 - 1123
