反应详情

To a mixture of 0.54 g (0.013 mol, 2.0 equiv) of 60% sodium hydride/mineral oil dispersion in 10 m of dry DMF was added dropwise at room temperature a solution 1.02 g (0.0067 mol) of the phenylacetic acid in 2.3 mL of DMF. After 15-20 minutes, a solid existed which was difficult to stir. The pyridazine (1.0 g, 0.0067 mol) was then added and the mixture was heated at 60°-65° C. for about 2 hours and was allowed to cool. The mixture was poured onto ice water and was adjusted to pH 5 with 2.0N HCl, and the precipitate was collected. This material was triturated under heptane to afford 880 mg of the title product. MP 124°-127° C.

1. temperaturethe mixture was heated at 60°-65° C. for about 2 hours
2. temperatureto cool
3. additionThe mixture was poured onto ice water
4. customthe precipitate was collected
5. customThis material was triturated under heptane