Yield:98027-52-2 91%

Reaction Conditions:

with triethylamine in dichloromethane at 0 - 20;

Steps:

12

l-(4-iodo-lH-pyrazol-l-yl)ethanoneAcetyl chloride (38.2 mL, 1.07 equiv) and triethylamine (86 mL, 1.2 equiv) were added at 0°C to a solution of 4-iodo-lH-pyrazole (lOOg, 0.515 mol) in dichloromethane (1 L). The mixture was stirred overnight at room temperature. The reaction mixture was poured into water. The aqueous layer was extracted with dichloromethane. The combined organic layers were washed with brine, dried over anhydrous sodium sulfate (Na₂S0₄), and filtered. The residue obtained byconcentration was purified by silica gel column chromatography (Hexane/EtOAc 20: 1 to 1 : 1) to give N-acetyl 4-iodo-lH-pyrazole as a solid (1 lOg, 91%).

References:

WO2012/118782,2012,A1 Location in patent:Page/Page column 107