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
- 0 °C
PROCEDURE
实验过程
In a 100 ml round bottom flask, 1-[2-fluoro-5-bromobenzyloxy]-3-[1-(t-butoxycarbonyl)piperidin-3-yl]propane (0.395 g) was dissolved in methylene chloride (4.2 ml). The solution was cooled to 0° C. and trifluoroacetic acid (0.8 ml) was slowly added dropwise. The resulting mixture was stirred at 0° C. for thirty minutes, followed by stirring at ambient temperature for thirty minutes. The progress of the reaction was monitored by thin layer chromatography. The reaction mixture was partitioned between 1 M potassium carbonate and methylene chloride. The aqueous fraction was back extracted with methylene chloride. The organic fractions were combined, and dried over sodium sulfate. The solvents were removed in vacuo. The desired title intermediate was further purified by liquid chromatography.
WORKUP
后处理
- stirringby stirring at ambient temperature for thirty minutes
- customThe reaction mixture was partitioned between 1 M potassium carbonate and methylene chloride
- extractionThe aqueous fraction was back extracted with methylene chloride
- dry with materialdried over sodium sulfate
- customThe solvents were removed in vacuo
- customThe desired title intermediate was further purified by liquid chromatography