HRID1105533
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was refluxed for 3 hours
- stirringwith stirring
- concentrationThe reaction mixture was concentrated
- addition5 ml of n-hexane was added to the
- concentrationconcentrate
- customto crystallize it
- filtrationThe resulting crystals were collected by filtration
- washwashed with n-hexane
- customdried