HRID1173870
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 (111 mg) obtained in Example 32-1 was dissolved in anhydrous methanol (1.0 ml) and then added with a 4 mol/l hydrogen chloride/dioxane solution (3.0 ml) and stirred at room temperature for 1 hour. After completion of the reaction, the solvent was distilled off and the residue was added with a 1 mol/l sodium hydroxide aqueous solution, followed by washing with dichloromethane. The aqueous layer was evaporated to dryness, followed by distilling azeotropically with chloroform. Consequently, the subject compound (48.5 mg) was obtained as a yellow oily substance.
WORKUP
后处理
- customAfter completion of the reaction
- distillationthe solvent was distilled off
- additionthe residue was added with a 1 mol/l sodium hydroxide aqueous solution
- washby washing with dichloromethane
- customThe aqueous layer was evaporated to dryness
- distillationby distilling azeotropically with chloroform