Dimethyl Sulfate → HCID 12665764, compound

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Reaction Steps

Dimethylsulfate (30 g, 0.22 mole) is added to a stirred solution of 1-methyl-5-chloro-3-phenylpyrazole (39.5 g, 0.2 mole) in dry xylene (350 ml) and the reaction mixture is warmed to 105°C to 115°C for 18 hours. A brown syrup separates out, the reaction is cooled and the xylene is decanted off. Dry acetone (300 ml) is added and after stirring a white precipitate separates out and is filtered off, m.p. 100°C to 102°C 33.8 g (55%). Recrystallization from dry acetone-toluene gives white needles m.p. 102°C to 104°C.

Provenance & Evidence