Реакция #11935

Уравнение реакции

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

Растворители

methanol

Условия реакции

Обработка

1. 1
   ДругоеAfter the reaction
2. 2
   Другоеthe solvent was removed by distillation
3. 3
   ДругоеThe 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
   Концентрированиеconcentrated
6. 6
   workup.DISTILLATIONazeotropically distilled with water
7. 7
   ПромывкаThe resulting solid was washed with ether

Методика

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.

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