Ammonia → HCID 23130733, compound

Participants

Reaction Steps

To a mixture of 2-amino-N-(5-phenoxy-thiophen-2-ylmethyl)-6-vinyl-nicotinamide described in Example A-168 (6.0 mg, 0.017 mmol) and toluene (0.5 mL) were added diiodine methane (0.0055 mL, 0.068 mmol) and diethyl zinc (1.1M toluene solution, 0.046 mL, 0.051 mmol) on an ice bath, and the solution was stirred at room temperature for 30 minutes. Water, ethyl acetate and an aqueous solution of 29% ammonia were added to the reaction solution for extraction, the organic layer was then washed with brine. The organic layer was evaporated in vacuo, then, residue was purified by reverse phase high performance liquid chromatography (acetonitrile-water mobile phase (containing 0.1% trifluoroacetic acid) was used), and trifluoroacetic acid salt of the title compound (0.40 mg, 0.00083 mmol, 4.9%) was obtained.

Provenance & Evidence