1: 1,1,1,2,2,2-hexabutyl-distannane With n-butyllithium in tetrahydrofuran; hexane T=-78°C; 1.16667 h; 2: 3-ethoxy-2-cyclopenten-1-one in tetrahydrofuran; hexane T=-78°C; 1.5 h; 3: With water in tetrahydrofuran; hexane T=-78 - 20°C;
in tetrahydrofuran a cold (-20°C) soln. of the cuprate reagent was allowed to react with β-iodo enone in dry THF; the mixt. was stirred under dry Ar atm. at -20°C for 15 min and at room temp. for 30 min;; the slurry was filtered through a column of Florisil, which was eluted with diethyl ether; column chromy. on silica gel, elution with 1:9 mixt. of diethyl ether-petroleum ether, distn. (air-bath temp. 150-154°C/0.2 Torr); elem. anal.;
参考文献
Piers, Edward; Morton, Howard E.; Chong, J. Michael
Canadian Journal of Chemistry, 1987 , vol. 65, p. 78 - 87