Jeon, Jong Yeob; Varghese, Jobi Kodiyan; Park, Ji Hae; Lee, Suck-Hyun; Lee, Bun Yeoul
European Journal of Organic Chemistry, 2012 , # 19 p. 3566 - 3569
in tetrahydrofuran; ethylene glycol dimethyl ether soln. of Ti(CO)3(dmpe)2 in DME stirred under CO for 3 h and then cooled to 0°C; cooled soln. of Na(DME)C5H5 in THF added; mixt. warmed to room temp.; CO replaced by Ar atmosphere; addn. of Et4NBr; filtration, removal of solvents and dmpe in vac.; cryst. product washed with ethanol (0°C) and dried in vac.;
参考文献
Chi,K.M.; Frerichs,S.R.; Kelseystein,B.
Journal of the American Chemical Society, 1988 , vol. 110, p. 163
in ethylene glycol dimethyl ether soln. of Ti(CO)3(dmpe)2 in DME stirred under CO at room temp. for 3 h; addn. of Na(DME)(C9H7) in DME at -30°C; soln. slowly warmed to room temp. over a period of 12 h; addn. of Et4NBr; slurry stirred for further 12 h; filtration, redn. of vol., addn. of diethyl ether; ppt. washed with ether and dried in vac.;
参考文献
Chi,K.M.; Frerichs,S.R.; Kelseystein,B.
Journal of the American Chemical Society, 1988 , vol. 110, p. 163
in ethylene glycol dimethyl ether soln. of Ti(CO)3(dmpe)2 in DME stirred under CO for 3 h; addn. of K(HBpz3) in DME; after 3 h addn. of Et4NBr; stirring continued for 6 h; filtration, solvent removed in vac. at room temp.; resulting solid washed with toluene, ethanol, and ether; recrystn. from acetonitrile/toluene; elem. anal.;
参考文献
Chi,K.M.; Frerichs,S.R.; Kelseystein,B.
Journal of the American Chemical Society, 1988 , vol. 110, p. 163
NOBF4 multistep r., 1.) CH2Cl2, -78 deg C, 2 h; 2.) CH2Cl2, CH3CN, r.t., 1 h; nitrosation products depend on reaction conditions and type of the nucleophile; Product distribution;