HRID11868
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 54-3 (7.2 mg) was dissolved in methanol (0.15 ml) and 4 mol/l hydrochloric acid/dioxane solution (0.15 ml) was added. After 2 hours, the reaction solution was concentrated. The residue was purified by silica gel column chromatography (chloroform/methanol/water=7/3/0.5). After the addition of 1 mol/l hydrochloric acid, the residue was concentrated and subjected to azeotropic distillation with methanol to obtain hydrochloride of the title compound (6.3 mg) as a white solid.
WORKUP
后处理
- concentrationthe reaction solution was concentrated
- customThe residue was purified by silica gel column chromatography (chloroform/methanol/water=7/3/0.5)
- additionAfter the addition of 1 mol/l hydrochloric acid
- concentrationthe residue was concentrated
- distillationsubjected to azeotropic distillation with methanol