Sulfuric Acid → HCID 12388581, compound

Participants

Reaction Conditions

Reaction Steps

81.4 g of 2-(p-tolyl)-4-hydroxy-2H-1,2,3-triazole-1-oxide (m.p. 150°-154° C. with decomp., prepared in accordance with Synthesis 1974 (March), pp. 198-199) are dissolved in 810 ml of dimethyl formamide at room temperature. Then 141.3 g of potassium carbonate are suspended in this solution and 48.3 ml of methyl iodide are poured into the suspension with good stirring. The batch is then heated to 60° C. over 30 minutes and kept thereat for 6 hours. The fine suspension is thereafter poured into 6 liters of water, and the pH is adjusted to 4-5 with 2N sulphuric acid. After cooling to room temperature, the solid is collected with suction, washed with water and dried to yield 56.5 g of 2-(p-tolyl)-4-methoxy-2H-1,2,3-triazole-1-oxide with a melting point of 62°-64° C. After recrystallisation from alcohol/water the product melts at 70°-72° C.

Provenance & Evidence