HRID377268

反应详情

EQUATION

反应方程式

HRID 377268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
4 °C

PROCEDURE

实验过程

3-(4-Piperidinopiperidinocarbonyl)propionic acid (0.26 g, 0.97 mmol) and DCC (0.25 g, 1.2 mmol) were dissolved in methylene chloride, followed by the addition of 4-nitrothiophenol (0.23 g, 1.2 mmol). The resulting mixture was stirred for 16 hours at 4° C. and then overnight at room temperature. The reaction mixture was filtered. After the filtrate was concentrated, the residue was purified by chromatography on a silica gel column (chloroform-acetone mixed solvent [10:1→5:1], whereby S-4-nitrophenyl 3-(4-piperidinopiperidinocarbonyl)propanethioate (196 mg, 50%) was obtained.

WORKUP

后处理

  1. customovernight
  2. customat room temperature
  3. filtrationThe reaction mixture was filtered
  4. concentrationAfter the filtrate was concentrated
  5. customthe residue was purified by chromatography on a silica gel column (chloroform-acetone mixed solvent [10:1→5:1]