HRID550588
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 130 °C
PROCEDURE
实验过程
3-Amino-6-methyl-pyrazine-2-carboxylic acid ethyl ester (Example C) (800 mg, 4.4 mmol) and 3-iodopyridine (1.63 g, 8.0 mmol) were dissolved in 17 ml dry dioxane. 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (510 mg, 0.88 mmol), cesium carbonate (2.30 g, 7.0 mmol) and tri(dibenzylideneacetone)dipalladium chloroform complex (460 mg, 0.44 mmol) were added and the reaction mixture was stirred for 16 hours at 130° C. The reaction mixture was then evaporated and purified by flash chromatography on silica gel (heptane/ethyl acetate 9:1->heptane/ethyl acetate 1:2). The desired product was obtained as a yellow oil (455 mg, 40%), MS: m/e=259.2 (M+H+).
WORKUP
后处理
- customThe reaction mixture was then evaporated
- custompurified by flash chromatography on silica gel (heptane/ethyl acetate 9:1->heptane/ethyl acetate 1:2)