HRID651431

反应详情

EQUATION

反应方程式

HRID 651431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.30 g of 2,6-dichloro-4-chloromethylpyridine and 0.25 g of tert-butyldimethylsilyl chloride were added to 4.0 ml of dimethylformamide, and were dissolved. The solution was cooled in an ice bath. After 0.14 g of imidazole was added, stirring was conducted at room temperature for 5.5 hours. Ethyl acetate was added to the reacted solution. The organic phase was washed with water, and was dried by adding sodium sulfate. The solvent was removed by evaporation, and the residue was purified by silica gel column chromatography to obtain 0.41 g of 2,6-dichloro-4-((1,1-dimethylethyl)dimethylsilyl)oxymethylpyridine (Compound No. 96).

WORKUP

后处理

  1. dissolutionwere dissolved
  2. temperatureThe solution was cooled in an ice bath
  3. washThe organic phase was washed with water
  4. customwas dried
  5. additionby adding sodium sulfate
  6. customThe solvent was removed by evaporation
  7. customthe residue was purified by silica gel column chromatography