Production of [11C]chloroform by direct chlorination of [11C]methane without catalyst support for the synthesis of [11C]diazomethane

The preparation of [11C]chloroform by direct chlorination of [11C]methane using gaseous chlorine by variation of temperature and reaction time (inert gas flow) without catalyst support for the online production of [11C]diazomethane in a flow-through synthesis apparatus is described in this work. At an oven temperature of 400 °C and a He flow of 50 mL/min, [11C]chloroform was synthesized inside a quartz glass column in a radiochemical yield of 31±2% with respect to [11C]methane. The online preparation of [11C]diazomethane by reaction of [11C]chloroform with hydrazine in an ethanolic KOH solution with small amounts of 18-crown-6-crownether succeeded with a radiochemical yield of 20±3% with respect to [11C]methane. The product [11C]diazomethane was measured indirectly in the form of 4-nitrobenzoic acid[11C]methylester using the esterification of 4-nitrobenzoic acid as a monitor reaction.