反应 #11964
ord-7d03949ae1e54900937fdaebc8008d05
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浓缩the reaction solution was concentrated
- 2其他The residue was purified by silica gel column chromatography (chloroform/methanol/water=7/3/0.5)
- 3workup.ADDITIONAfter the addition of 1 mol/l hydrochloric acid
- 4浓缩the residue was concentrated
- 5workup.DISTILLATIONsubjected to azeotropic distillation with methanol
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.