This invention belongs to the field of cycloazinone preparation technology, and provides a high-yield cycloazinone synthesis process, including the following steps: Step 1: N-ethoxycarbonyl-N,N,N-trimethylguanidine and a
solid-phase catalyst are added to
toluene and stirred evenly. Under
nitrogen protection, the temperature is raised to 40-60°C, and a cyclohexyl
isocyanate toluene solution is added dropwise. Stirring is continued for 2-4 hours. The
solid-phase catalyst is recovered by
filtration, and the mixture is concentrated under reduced pressure to obtain N-cyclohexylcarbamoyl-N-ethoxycarbonyl-N,N,N-trimethylguanidine; Step 2: Under
nitrogen protection, the temperature is raised to 50-60°C, and the N-cyclohexylcarbamoyl-N-ethoxycarbonyl-N,N,N-trimethylguanidine
toluene solution is added dropwise to a
sodium methoxide toluene solution and stirred for 1-2 hours. The temperature is lowered to
room temperature, and glacial
acetic acid is added for
neutralization. After washing, the mixture is concentrated under reduced pressure, and a crystallizing agent is added. The temperature is lowered to 0-5°C, and the mixture is stirred for
crystallization for 2-4 hours. After
filtration and washing, the mixture is dried under vacuum to obtain the finished cycloazinone.