HRID2070602

反应详情

EQUATION

反应方程式

HRID 2070602 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. stirringby stirring the mixture at 90° C. for 1.5 hours
  2. filtrationThe reaction mixture was filtered through Celite
  3. concentrationthe filtrate was concentrated
  4. customThe residue was purified by column chromatography on silica gel (ethyl acetate:hexane (volume ratio)=1:49 to 1:9)