Methyl Isocyanate → 1-Piperazinecarboxamide, N-methyl-N-((methylamino)carbonyl)-4-(3-(trifluoromethyl)phenyl)-

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Reaction Steps

Into 70 ml of dichloromethane, was dissolved 4.3 g of 1-(methylcarbamoyl)-4-(m-trifluoromethylphenyl)piperazine and 0.9 g of methyl isocyanate. To the solution, while being stirred and cooled in ice, was added dropwise 3.9 g of anhydrous stannic chloride. After 15 hours of reaction at room temperature, the precipitated matter was collected by filtration and stirred in a mixture of dichloromethane and water. The organic layer was separated and dried over anhydrous sodium sulfate. After removal of the solvent by distillation, the residue was recrystallized from a mixture of ethanol and petroleum ether to obtain 3.2 g (62% yield) of 1-(2,4-dimethylallophanoyl)-4-(m-trifluoromethylphenyl)piperazine.

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