Iodoethane → HCID 12813183, compound

Participants

Reaction Steps

A 4 gram portion of 1,4-bis-(α,α,α-trifluoro-3-tolyl)-3-pyrazolin-5-one (from Example 4) was heated with 20 ml. ethyl iodide, 3 grams potassium carbonate, and 40 ml. ethanol at reflux temperature for about 4 hours. The reaction product mixture was concentrated in vacuo and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, the drying agent filtered off and the filtrate concentrated in vacuo. On standing overnight the residue solidified and was recrystallized from a mixture of hexane and benzene. The solid was chromatographed on a silica gel column using a mixture of ethyl acetate and hexane in the ratio of 1:2. The product from the column was then recrystallized from a mixture of hexane and benzene to yield the desired product, m.p. 110°-111° C.

Provenance & Evidence