HRID11849

反应详情

EQUATION

反应方程式

HRID 11849 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 12-5 (26.8 mg) was dissolved in methanol (0.5 ml), and 4 mol/l hydrochloric acid/dioxane solution (0.5 ml) was added. The mixture was stirred for 4.5 hours at room temperature. After the reaction, the solvent was removed by distillation. The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5). The obtained product was added with an aqueous solution of hydrochloric acid and concebtrated, and then azeotropically distilled with water. The resulting solid was washed with ether to obtain a hydrochloride of the title compound (25.8 mg) as a white solid.

WORKUP

后处理

  1. customAfter the reaction
  2. customthe solvent was removed by distillation
  3. customThe residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5)
  4. additionThe obtained product was added with an aqueous solution of hydrochloric acid
  5. distillationazeotropically distilled with water
  6. washThe resulting solid was washed with ether