hydrogenchloride in toluene condensing gaseous HCl with liquid nitrogen in an ampul containing toluene solution of (((CH3)3Si)2N)2Yb*CH3O(CH2)2OCH3; warming to room temperature; removing volatile compounds ((CH3)3SiCl, DME) by vac. condensation; vac. sublimation at 100°C (1E-2 mm): NH4Cl;;
参考文献
Journal of General Chemistry USSR (English Translation), , vol. 55, p. 1911 - 1914
Zhurnal Obshchei Khimii, , vol. 55, p. 2153 - 2157
a 6*molar excess of NH4Cl is added to Yb2O3 dissolved in HCl; the dried mixt. is confined in Pyrex and heated slowly under vac. for 2 d to ca. 400°C to remove first the coordinated water and then to decompose the resulting (NH4)3YbCl6;
参考文献
Journal of Solid State Chemistry, , vol. 74, # 1 p. 67 - 73
in neat (no solvent) absence of moisture; large excess AlCl3, evacuated quartz tube, 573 K; fractional sublimation over 450 to 650 K gradient, removal of residual AlCl3 on heating in Cl2/N2 stream;
