反应详情

温度

90 °C

A solution of 4-bromo-6-chloro-2-methylpyridazin-3(2H)-one (2.42 g, 10.8 mmol), tert-butyl 4-(6-aminopyridin-3-yl)piperidine-1-carboxylate (2.73 mg, 9.83 mmol), Xantphos (853 mg, 1.47 mmol) and cesium carbonate (9.61 g, 29.5 mmol) in dry dioxane (80 ml) was vacuum de-gassed and place under an argon atmosphere. To this mixture was added tris(dibenzylideneacetone)dipalladium (0) (203 mg, 197 mmol) and the vacuum de-gas cycle was repeated. The material was heated at 90° C. (oil bath) with vigorous stirring overnight. The flask was cooled to ambient temperature and the contents were filtered through a plug of celite, rinsing well with dioxane, the filtrate concentrated and the resulting residue triturated with 1; 1 ratio of ether/ethyl acetate. This provided the desired product as an off-white powder (2.73 g, 71.2%). (M+H)+=420.2 m/e.

1. customde-gassed
2. customthe vacuum de-gas cycle
3. temperatureThe flask was cooled to ambient temperature
4. filtrationthe contents were filtered through a plug of celite
5. washrinsing well with dioxane
6. concentrationthe filtrate concentrated
7. customthe resulting residue triturated with 1