HRID1780611

反应详情

EQUATION

反应方程式

HRID 1780611 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 8.3 g of the 5-(2,3-dihydro-2,2,4,5,6-pentamethylbenzofuran-7-yl)cyclohexane-1,3-dione in 80 ml of absolute toluene was added 18 ml of anhydrous butyric acid and refluxed for 4 hours. The reaction mixture was concentrated under reduced pressure to afford a residue. To the solution of the residue in 100 ml of toluene was added 1.6 g of dimethylaminopyridine. After refluxing for 15 hours, the reaction mixture was cooled to room temperature and concentrated under reduced pressure to afford a crude product. Final purification was carried by silica-gel column chromatography to afford 6.1 g of 2-butyryl-5-(2,3-dihydro-2,3,4,5,6-penta-methylbenzofuran-7-yl)-3-hydroxycyclohex-2-en-1-one as a yellow solid.

WORKUP

后处理

  1. temperaturerefluxed for 4 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customto afford a residue
  4. temperatureAfter refluxing for 15 hours
  5. concentrationconcentrated under reduced pressure
  6. customto afford a crude product
  7. customFinal purification