HRID1105533

反应详情

EQUATION

反应方程式

HRID 1105533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The compound (57.3 mg) obtained in Example 5 was dissolved in 10 ml of benzene, and with stirring at room temperature, 0.5 ml of thionyl chloride was added. The mixture was refluxed for 3 hours with stirring. The reaction mixture was concentrated, and 5 ml of n-hexane was added to the concentrate to crystallize it. The resulting crystals were collected by filtration, washed with n-hexane and dried to afford 34.8 mg of the desired product.

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 3 hours
  2. stirringwith stirring
  3. concentrationThe reaction mixture was concentrated
  4. addition5 ml of n-hexane was added to the
  5. concentrationconcentrate
  6. customto crystallize it
  7. filtrationThe resulting crystals were collected by filtration
  8. washwashed with n-hexane
  9. customdried