Picryl chloride can be prepared from pyridine picrate and either phosphorus oxychloride or phosgene in 97 to 100% yield. The pyridine used in this process is recoverable as its picrate and thus acts as a non-expended carrier during repeated preparations. Two of the chlorine atoms react in phosphorus oxychloride while only one in phosgene furnishes picryl chloride. The latter acid chloride is, however, more economical in use owing to its lower cost and molecular weight.