Low-water-content diazomethane-d2 and its isotopic assay

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 present in any solution of diazomethane could be determined by a GC-MS analysis and 1H NMR spectrometry on a suitable derivative. In addition, a procedure for the quantitative determination of water in diazomethane solutions has been developed. (author)