反应详情

6-Chloronicotinoyl chloride (500 mg, 2.84 mmol) and acetohydrazide (232 mg, 3.12 mmol) were added to dimethylformamide (14.2 mL) at 0° C. The mixture was allowed to warm to room temperature and maintained at room temperature overnight. The reaction was then slightly concentrated in vacuo and diluted in acetonitrile. This mixture was directly purified via reverse phase HPLC (10-100% acetonitrile/water+0.05% TFA modifier). Fractions containing the desired product were lyophilized and free based using bicarbonate resin to afford the title compound.

1. temperaturemaintained at room temperature overnight
2. concentrationThe reaction was then slightly concentrated in vacuo
3. additiondiluted in acetonitrile
4. customThis mixture was directly purified via reverse phase HPLC (10-100% acetonitrile/water+0.05% TFA modifier)
5. additionFractions containing the desired product