Methyl iodide → HCID 15586382, compound

Participants

Reaction Steps

A hot solution of 2,5-dimethyl-6-phenyl-1,2,4-triazin-3(2H)-one (5 g) in benzene (60 ml) was added dropwise to a stirred solution of methylmagnesium iodide prepared from methyl iodide (17.5 g) and magnesium turnings (3 g) in diethyl ether (80 ml) at room temperature. The solution was refluxed under heating for 40 minutes and then allowed to stand for 1 hour at room temperature. The solution was treated with a saturated aqueous solution of ammonium chloride to decompose excess Grignard reagent. The organic layer was separated, dried over magnesium sulfate, treated with activated charcoal, and evaporated to dryness. The resultant solid was recrystallized from a mixture of diispropyl ether and chloroform to give 6-phenyl-2,5,5-trimethyl-4.5-dihydro-1,2,4-triazin-3(2H)-one (4.21 g), m.p. 128°~130° C.

Provenance & Evidence