反応 #11963
ord-2bfa4290bd144e32ab8ac973d4d7ed90
反応方程式
反応物
試薬
なし
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1濃縮the reaction solution was concentrated
- 2workup.DISTILLATIONazeotropically distilled with methanol
- 3その他The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5)
実験手順
The compound obtained in Example 53-3 (19.0 mg) was dissolved in methanol (0.19 ml) and 4 mol/l hydrochloric acid/dioxane (0.19 ml) was added. After 2.5 hours, the reaction solution was concentrated and azeotropically distilled with methanol. The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5). The obtained title compound was dissolved in methanol. Activated carbon (4 mg) was added to the solution, followed by filtration and concentration. After the addition of 1 mol/l hydrochloric acid and a small amount of methanol, the residue was concentrated and dried under reduced pressure to obtain hydrochloride of the title compound (17.9 mg) as a yellow solid.