Reacción #11935

Ecuación de reacción

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

Disolventes

methanol

Condiciones de reacción

Tratamiento posterior

1. 1
   OtroAfter the reaction
2. 2
   Otrothe solvent was removed by distillation
3. 3
   OtroThe 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
   Concentraciónconcentrated
6. 6
   workup.DISTILLATIONazeotropically distilled with water
7. 7
   LavadoThe resulting solid was washed with ether

Procedimiento

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.

Fuente