sodium hydride in isopropyl alcohol; benzene (Ar); excess of NaH and dry isopropanol stirred for ca. 0.5 h, soln. of semicarbazone in C6H6 added slowly, mixt. refluxed for 2.5 h, mixt. cooled to room temp., soln. of tin-compound in C6H6 added dropwise, mixt. refluxed for 2 h; mixt. filtered, filtrate evapd. (reduced pressure, rotary evaporator), recrystd. from 2:1 mixt. of benzene and petroleum ether at 40-60 °C; elem. anal.;
参考文献
Singh
Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry, 2003 , vol. 33, # 10 p. 1895 - 1909
sodium hydride in isopropyl alcohol; benzene (Ar); excess of NaH and dry isopropanol stirred for ca. 0.5 h, soln. of semicarbazone in C6H6 added slowly, mixt. refluxed for 2.5 h, mixt. cooled to room temp., soln. of tin-compound in C6H6 added dropwise, mixt. refluxed for 2 h; mixt. filtered, filtrate evapd. (reduced pressure, rotary evaporator), recrystd. from 2:1 mixt. of benzene and petroleum ether at 40-60 °C; elem. anal.;
参考文献
Singh
Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry, 2003 , vol. 33, # 10 p. 1895 - 1909
diethyl malonate in ethanol; toluene Na was dissolved in EtOH at room temp., diethylmalonate was added, toluene was added, acetyl chloride was added at room temp.; ppt. was centrifugated and washed with EtOH; powder X-ray diffraction;
platinum in not given reaction of Na2SO4 with NH4Cl in presence of platinum black; complete reaction on threefold or sixfold evaporating Na2SO4 with NH4Cl;;
参考文献
Ber., , vol. 59, p. 1340 - 1340
→
反应条件
lithium peroxide in neat (no solvent) byproducts: O2; NaClO4, Mg, Li2O2 mixed in agate mortar; heated in alundum crucibles at a heating rate of 10 K/min to 700°C;
参考文献
Russian Journal of Inorganic Chemistry, , vol. 51, # 9 p. 1349 - 1354
