Sodium Hydroxide → HCID 9920415, compound

Participants

Reaction Steps

167.7 g (2.36 mol) of chlorine were passed into a solution of 165 g (1.5 mol) of 1-ethyl-4-methylpyrazole and 625 g of 1,2-dichloroethane over the course of 2 h. The temperature rose to 60° C. and could be kept at 60° C. by cooling with ice. While cooling, the resulting reaction solution was neutralized at 25° C. with 533.9 g (2.0 mol) of 15% strength aqueous sodium hydroxide solution. After phase separation, the organic phase was distilled to afford 122.1 g (0.843 mol) of 5-chloro-1-ethyl-4-methylpyrazole of boiling point (200) 118° C. and a purity of 99.8% (GC) and 109.1 g (0.61 mol) of 3,5-dichloro-1-ethyl-4-methylpyrazole of boiling point (200) 154° C. and a purity of 99.6%. This corresponds to a yield of 96.6% of theory based on 1-ethyl-4-methylpyrazole.

Provenance & Evidence