反应 #11940
ord-f9b2fbe11f024165adc3b05c701f2695
反应方程式
反应物
试剂
无
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他After the reaction
- 2其他the solvent was removed by distillation
- 3其他The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5)
- 4workup.ADDITIONThe obtained product was added with an aqueous solution of hydrochloric acid
- 5浓缩concentrated
- 6workup.DISTILLATIONazeotropically distilled with water
- 7洗涤The resulting solid was washed with ether
实验过程
The compound obtained in Example 11-5 (30.6 mg) was dissolved in methanol (0.7 ml), and 4 mol/l hydrochloric acid/dioxane solution (0.7 ml) was added. The mixture was stirred for 3 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, concentrated and then azeotropically distilled with water. The resulting solid was washed with ether to obtain a hydrochloride of the title compound (22.7 mg) as a white solid.