反応 #11935

反応方程式

compound

(2S)-2-(4-(N-Boc-N-2-picolylaminomethyl)phenylacetyl)amino-5-(5,6,7,8-tetrahydroquinolin-8-yl)aminovaleric acid

hydrochloric acid dioxane

→

hydrochloride

title compound

(2S)-2-((4-(N-2-picolylaminomethyl)phenylacetyl)amino)-5-(5,6,7,8-tetrahydroquinolin-8-yl)aminovaleric acid

溶媒

methanol

反応条件

後処理

1. 1
   その他After the reaction
2. 2
   その他the solvent was removed by distillation
3. 3
   その他The residue was purified by silica gel column chromatography (1.0 g, chloroform/methanol/water=7/3/0.5)
4. 4
   workup.ADDITIONThe obtained product was added with an aqueous solution of hydrochloric acid
5. 5
   濃縮concentrated
6. 6
   workup.DISTILLATIONazeotropically distilled with water
7. 7
   洗浄The resulting solid was washed with ether

実験手順

The compound obtained in Example 8-8 (18.0 mg) was dissolved in methanol (0.2 ml) and 4 mol/l hydrochloric acid/dioxane solution was added. The mixture was stirred for 1.5 hours at room temperature. After the reaction, the solvent was removed by distillation. The residue was purified by silica gel column chromatography (1.0 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 (14.4 mg) as a white solid.

出典