Thionyl Chloride → HCID 13281458, compound

Participants

Reaction Steps

A solution of 4-cyano-5-(2-hydroxyethyl)amino-1-(2,3,4-trichlorophenyl)pyrazole (3.0 g; prepared as described in Example 27) in thionyl chloride (25 ml) was heated under reflux for 5 hours. The solution was evaporated under reduced pressure and the residue was dissolved in dichloromethane (100 ml). The dichloromethane solution was washed with water (2×200 ml), dried over anhydrous magnesium sulphate and evaporated to give an orange gum, whicn was chromatographed using dichloromethane as eluent. Evaporation of the eluate containing the major component gave 5-(2-chloroethyl)amino-4-cyano-1-(2,3,4-trichlorophenyl)pyrazole, m.p. 125°-128° C., in the form of a cream-coloured solid.

Provenance & Evidence