Ethyl chloroformate → HCID 11421894, compound

Participants

Reaction Conditions

Reaction Steps

Sodium hydride (0.012 g, 0.3 mmol) was added to a solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-[N-(2-hydroxyethyl)-N-methylamino]-4-trifluoromethylsulfonylpyrazole (0.100 g, 0.2 mmol) in dry tetrahydrofuran, and stirred under an atmosphere of nitrogen for 2 hours at 20° C. Ethyl chloroformate (0.029 g, 0.3 mmol) was added and stirring continued for 1 hour at 20° C. The mixture was then added to saturated ammonium chloride solution and ethyl acetate, and the organic layer washed with water and brine, dried (sodium sulfate), and evaporated. The residue was purified by flash column chromatography eluting with heptane/ethyl acetate (4:1) to give the title compound as a white powder (0.098 g, Compound 6, yield: 81%), 19F-NMR: −63.8, −78.6.

Provenance & Evidence