HRID2240185

反应详情

EQUATION

反应方程式

HRID 2240185 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2-(3-fluorobenzoyl)-4-methoxybenzoyl chloride (3.36 g) and piperidin-3-one hydrochloride (1.88 g) in 54 ml of toluene was added 2,6-lutidine (4.01 ml). The reaction was heated at reflux (3:10 pm) for 24 h, then partitioned between EtOAc and 400 mL of 1 N HCl. The aqueous solution was extracted twice more with EtOAc. The combined organic solutions were dried (MgSO4) and concentrated. Flash chromatography (40-100% EtOAc/hexanes) to gave the titled compound.

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureat reflux (3:10 pm) for 24 h
  3. custompartitioned between EtOAc and 400 mL of 1 N HCl
  4. extractionThe aqueous solution was extracted twice more with EtOAc
  5. dry with materialThe combined organic solutions were dried (MgSO4)
  6. concentrationconcentrated