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
PROCEDURE
实验过程
To a mixture of palladium(II) acetate (135 mg), 2-(di-tert-butylphosphino)-1,1′-binaphthyl (478 mg) and cesium carbonate (3.9 g) was added toluene (15 mL), followed by stirring under argon atmosphere at room temperature for 10 minutes. To this reaction mixture were added spiro[4.5]dec-7-yl-methanol (1.0 g) obtained in Step 1 and 6-bromopyridine-3-carboxaldehyde (1.1 g), followed by stirring the mixture at 90° C. for 1.5 hours. The reaction mixture was filtered through Celite and the filtrate was concentrated. The residue was purified by column chromatography on silica gel (ethyl acetate:hexane (volume ratio)=1:49 to 1:9) to give 6-(spiro[4.5]dec-7-ylmethoxy)-pyridine-3-carboxaldehyde (0.313 g).
WORKUP
后处理
- stirringby stirring the mixture at 90° C. for 1.5 hours
- filtrationThe reaction mixture was filtered through Celite
- concentrationthe filtrate was concentrated
- customThe residue was purified by column chromatography on silica gel (ethyl acetate:hexane (volume ratio)=1:49 to 1:9)