Preparation of 3-nitrobenzenediazonium perchlorate
Alternative Names: 3-nitrobenzenediazonium perchlorate; m-nitrobenzenediazonium perchlorate; meta-nitrobenzenediazonium perchlorate
0.5 g of m-nitroaniline is suspended in 5 ml of water, and 0.5 ml of concentrated hydrochloric acid and 2.2 ml of 20% perchloric acid solution are added. After the m-nitroaniline has dissolved, 15 ml of water is added and the solution is cooled by immersing the solution in a beaker filled with a slurry of cracked ice. One-quarter of a gram of sodium nitrite dissolved in 1 or 2 ml of water is added in 3 or 4 portions, the mixture being shaken after each addition or stirred with a stirring rod the end of which is covered with a short piece of rubber tubing. After standing in the cold for 5 minutes, the material is transferred to a filter, and the feltlike mass of pale yellow needles is washed with cold water, with alcohol, and with ether. The product is dried in several small portions on pieces of filter paper.
Chemistry of Powder and Explosives, by T. L. Davis, 443, 1941