butyllithium; CH2Cl2 in tetrahydrofuran; diethyl ether; benzene Li(PyPhCH) in THF (prepd. in situ) added dropwise over 30 min to stirred suspn. of PdCl2(γmpy) in ether at -80°C under N2; warmed to room temp.; benzene added; soln. 1 h heated to 60°C (ether distd.); cooled deep red soln. hydrolysed; organic phase isolated, filtered, dried over MgSO4, reduced to dryness in vac.; red orange gum extd. with hot hexane; remaining gum dissolved in CH2Cl2; acetone added; orange crystals sepd. by slow evapn. (20 h); elem. anal.;
参考文献
Australian Journal of Chemistry, , vol. 41, p. 651 - 666
butyllithium in tetrahydrofuran; diethyl ether; benzene Li(PyPhCH) in THF (prepd. in situ) added dropwise over 30 min to stirred suspn. of PdCl2(γmpy) in ether at -80°C under N2; warmed to room temp.; benzene added; soln. 1 h heated to 60°C (ether distd.); cooled deep red soln. hydrolysed; org. phase isolated, dried, reduced to dryness; red orange gum chromd. on SiO2 (Et acetate/CHCl3); first orange fraction Pd((PyPhC)C(Me)O)2 recrystd. (acetone/CH2Cl2); (Pd(PyPhCH)(γmpy)Cl)2 isolable from retaining material on column; elem. anal.;
参考文献
Australian Journal of Chemistry, , vol. 41, p. 651 - 666
in water T=180°C; 120 h; sealed ampule; Mechanism;
参考文献
Chemistry of Heterocyclic Compounds (New York, NY, United States), , vol. 19, # 9 p. 970 - 976
Khimiya Geterotsiklicheskikh Soedinenii, , # 9 p. 1214 - 1221
Tschitschibabin; Kuindshi; Benewolenskaja
Chemische Berichte, 1925 , vol. 58, p. 1585
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Koenigs; Koehler; Blindow
Chemische Berichte, 1925 , vol. 58, p. 938
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Koenigs; Mensching; Kirsch
Chemische Berichte, 1926 , vol. 59, p. 1720
