Silver hyponitrite is the starting material for the synthesis of alkyl hyponitrites, which are useful low-temperature sources of alkoxy radicals. l-5 Numerous syntheses of sodium and silver hyponitrites have appeared in the literat~ re-j-~ Most are tedious, hazardous, poorly described, or require large quantities of mercury. In our hands, one procedure gave no product and the reaction mixture from another ignited during work-up. The method ...