Triethylamine → HCID 58443700, compound

Participants

Reaction Steps

To a stirred solution of O-methyl-N-[3-(2,4,6-trichloro-phenyl)-propyl]-hydroxylamine (0.35 g, 1.3 mmol) prepared as described in example P24c in dichloromethane (5 ml), triethylamine (0.55 ml, 3.9 mmol) and a solution of 3-difluoromethyl-1-methyl-1H-pyrazole-4-carbonyl chloride acid in dichloromethane (2 ml) was added slowly at a temperature of 0° C. After complete addition of the acid chloride the mixture was stirred at ambient temperature for the next 3 hours. When the TLC confirmed the completion of the reaction, the reaction mass was diluted with water and extracted with dichloromethane (3×60 ml). The combined dichloromethane layer was washed with 2N HCl followed by saturated NaHCO3 solution, water and finally brine. The organic layer was then dried over anhydrous sodium sulphate and concentrated under reduced pressure. The resulting crude mass was purified over column chromatography (silica gel 60-120 mesh, 26% ethylacetate in hexane) to afford 3-Difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid methoxy-[3-(2,4,6-trichloro-phenyl)-propyl]-amide (0.5 g, 91%) as white crystalline solid. m.p-95-96° C.

Provenance & Evidence