Potassium Carbonate → HCID 10498867, compound

Participants

Reaction Steps

3 g of N-diaminomethylene-2-ethyl-4-chloro-5-methylsulfonylbenzamide [obtainable by reacting methyl 2-methyl-4-chloro-5-methylsulfonylbenzoate with guanidine] are heated with 30 ml of 4-trimethylsilyloxypyridine in the presence of 3 g of K2CO3 in a closed tube at 135° for five hours. The mixture is cooled, the excess silylpyridine is removed by decanting, and the residue is triturated with ether and filtered off with suction. The solid residue is then dissolved in methanol and chromatographed over silica gel (ethyl acetate/methanol). Recrystallization from isopropanol and ethanol gives N-diaminomethylene-2-ethyl-4-(1,4-dihydro-4-oxo-1-pyridyl)-5-methylsulfonylbenzamide, m.p. 261-263°.

Provenance & Evidence