Reaktion #11940

Reaktionsgleichung

compound

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

hydrochloric acid dioxane

→

hydrochloride

title compound

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

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter the reaction
2. 2
   Sonstigethe solvent was removed by distillation
3. 3
   SonstigeThe residue was purified by silica gel column chromatography (1 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
   Einengenconcentrated
6. 6
   workup.DISTILLATIONazeotropically distilled with water
7. 7
   WaschenThe resulting solid was washed with ether

Vorschrift

The compound obtained in Example 11-5 (30.6 mg) was dissolved in methanol (0.7 ml), and 4 mol/l hydrochloric acid/dioxane solution (0.7 ml) was added. The mixture was stirred for 3 hours at room temperature. After the reaction, the solvent was removed by distillation. The residue was purified by silica gel column chromatography (1 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 (22.7 mg) as a white solid.

Quelle