HRID11868

反应详情

EQUATION

反应方程式

HRID 11868 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationthe reaction solution was concentrated
  2. customThe residue was purified by silica gel column chromatography (chloroform/methanol/water=7/3/0.5)
  3. additionAfter the addition of 1 mol/l hydrochloric acid
  4. concentrationthe residue was concentrated
  5. distillationsubjected to azeotropic distillation with methanol