Phosgene → HCID 20228142, compound

Participants

Reaction Conditions

Reaction Steps

18.6 g (0.1 mole) of 6-isopropyl-3-mercapto-4-methyl-1,2,4-triazin-5(4H)-one are suspended in 100 ml of ethyl acetate. Then 10.9 g (0.11 mole) of phosgene are introduced at room temperature. The ensuing reaction is slightly exothermic. As the reaction is not yet complete, the mixture is stirred for 1 hour at 45° C. The mixture, which is still in the form of a white suspension, is then filtered. The residue is washed with absolute diethyl ether and the resultant white powder is dried in vacuo without heating, affording 20.3 g (90.8% of theory) of 3-chloro-6-isopropyl-4-methyl-1,2,4-triazin-5(4H)-one hydrochloride with a melting point of 144° C. (dec.). The compound sublimes when heated to 45° C. in a high vacuum, yielding the free chloride with a melting point of 129° C. (dec.).

Provenance & Evidence