HRID963466

反应详情

EQUATION

反应方程式

HRID 963466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-adamantanone (2.00 g) in formic acid (10 ml) was added dropwise a suspension of hydroxyamine-O-sulfonic acid (2.26 g) in formic acid (7 ml) under stirring at ambient temperature. The mixture was heated at reflux temperature for 3.5 hours. The reaction mixture was allowed to cool to room temperature, alkalined with 1N sodium hydroxide aqueous solution and extracted with chloroform twice. The combined extracts were washed with water and dried over sodium sulfate. Removal of the solvent gave 2-azatricyclo[4.3.1.14,8 ]undecan-3-one (2.14 g), which was used in a following reaction step without further purification.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux temperature for 3.5 hours
  3. temperatureto cool to room temperature
  4. extractionextracted with chloroform twice
  5. washThe combined extracts were washed with water
  6. dry with materialdried over sodium sulfate
  7. customRemoval of the solvent