反应详情

温度

20 °C

A solution of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-4-methylsulfinylpyrazole (10 g) in dry DMF was added during 10 minutes to potassium hydride (0.7 g of a 35% suspension in oil) in dry DMF at 4° C. and stirred for 20 min. Vinyl ethyl sulfone (3.13 g) in dry DMF was added. over 5 hr at 4° C. and the mixture stirred overnight whilst warming to 20° C. under a nitrogen atmosphere. The mixture was recooled, ammonium chloride solution added and the organic layer washed (water), dried (sodium sulfate) and evaporated. The residue was crystallized (ethyl acetate/hexane) to give 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-(2-ethylsulfonylethylamino)-4-methylsulfinylpyrazole (4.08 g), m.p. 131-132° C.

1. waitover 5 hr at 4° C.
2. stirringthe mixture stirred overnight
3. washthe organic layer washed (water)
4. dry with materialdried (sodium sulfate)
5. customevaporated
6. customThe residue was crystallized (ethyl acetate/hexane)