Diethyl Ether → HCID 68824608, compound

Participants

Reaction Conditions

Reaction Steps

Title compound 8A, 3-(5-amino-4-cyanopyrazol-1-yl)benzoic acid (3.2 g, 1.0 eq, 14.04 mmol) was suspended in a toluene/methanol [3:1] solution (70 ml). This was then cooled to 0° C. and trimethylsilyldiazomethane was added drop wise as a 2M solution in diethyl ether (7.7 ml, 1.1 eq, 15.44 mmol). The reaction was allowed to warm to room temperature over 2 hours. A further portion of trimethylsilyidiazomethane (1.54 ml, 0.2 eq, 2.8 mmol) was added. The reaction was stirred at room temperature for a further 45 minutes and solvent was then removed in vacuo to give the title compound as an orange solid (3.4 g, 14.04 mmol, 100%). LCMS: [M+H]+=243, Rt=1.05 min, 100% purity.

Provenance & Evidence