HRID1849963

反应详情

EQUATION

反应方程式

HRID 1849963 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 2,2,6,6-tetramethylpyran-3,5-dione (741 mg, 4.35 mmol) in chloroform (10 ml) is added phosphorus pentachloride (454 mg, 2.18 mmol), and the reaction is heated to reflux for 5 hours. Silica gel is added to the cooled crude reaction mixture, the solvent is evaporated under reduced pressure and the residue is purified by flash chromatography on silica gel to give 5-chloro-2,2,6,6-tetramethyl-6H-pyran-3-one (349 mg).

WORKUP

后处理

  1. temperaturethe reaction is heated
  2. temperatureto reflux for 5 hours
  3. additionSilica gel is added to the
  4. temperaturecooled crude
  5. customreaction mixture
  6. customthe solvent is evaporated under reduced pressure
  7. customthe residue is purified by flash chromatography on silica gel