HRID1066837

反应详情

EQUATION

反应方程式

HRID 1066837 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringby stirring at ambient temperature for thirty minutes
  2. customThe reaction mixture was partitioned between 1 M potassium carbonate and methylene chloride
  3. extractionThe aqueous fraction was back extracted with methylene chloride
  4. dry with materialdried over sodium sulfate
  5. customThe solvents were removed in vacuo
  6. customThe desired title intermediate was further purified by liquid chromatography