HRID11843
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 obtained in Example 10-1 (13.9 mg) was dissolved in methanol (0.28 ml) and 4 mol/l hydrochloric acid/dioxane solution (0.28 ml) was added to the solution. The mixture was stirred for 75 minutes at room temperature. After the completion of the reaction, the solvent was removed by distillation. The residue was purified by silica gel column chromatography (0.5 g, chloroform/methanol/water=7/3/0.5). The obtained product was added with aqueous solution of hydrochloric acid, concentrated and then azeotropically distilled with water. The resulting solid was washed with ether to obtain a hydrochloride of the title compound (13.8 mg) as a white solid.
WORKUP
后处理
- customAfter the completion of the reaction
- customthe solvent was removed by distillation
- customThe residue was purified by silica gel column chromatography (0.5 g, chloroform/methanol/water=7/3/0.5)
- additionThe obtained product was added with aqueous solution of hydrochloric acid
- concentrationconcentrated
- distillationazeotropically distilled with water
- washThe resulting solid was washed with ether