HRID1748521

反应详情

EQUATION

反应方程式

HRID 1748521 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 8-(5-bromopyridin-2-yl)-1,4-dioxaspiro[4,5]decane-8-carboxylic acid (776 mg) in dimethylsulfoxide (3 ml) was stirred at 150° C. for 1.5 hours. After completion of the reaction, the reaction solution was left stand to room temperature, water was added and extracted with ethyl acetate. The organic solution was washed with water and saturated brine successively, dried over anhydrous sodium sulfate and concentrated. The resulting residue was purified with silica gel column chromatography (n-hexane/ethyl acetate) to give 5-bromo-2-(1,4-dioxaspiro[4,5]decane-8-yl)pyridine (646 mg) as a colorless oil.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. waitthe reaction solution was left stand to room temperature
  3. extractionextracted with ethyl acetate
  4. washThe organic solution was washed with water and saturated brine successively
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customThe resulting residue was purified with silica gel column chromatography (n-hexane/ethyl acetate)