P. Strazzolini et al., LOW-WATER-CONTENT DIAZOMETHANE-D(2) AND ITS ISOTOPIC ASSAY, Bulletin of the Chemical Society of Japan, 69(10), 1996, pp. 2943-2946
A multiple D2O-CH2N2 exchange followed by a final anhydrification with
K2CO3 gave an alcohol-free low-water-content ether solution of CD2N2.
Procedural improvements for the exchange are reported. The extent of
deuteration with a quantitative evaluation of the actual species prese
nt in any solution of diazomethane could be determined by a GC-MS anal
ysis and H-1 NMR spectrometry on a suitable derivative. In addition, a
procedure for the quantitative determination of water in diazomethane
solutions has been developed.