Reaktion #11964

Reaktionsgleichung

compound

(2S)-2-(4-(N-2-picolyl-N-Boc aminomethyl)naphthoylamino)-5-((8R)-5,6,7,8-tetrahydroquinolin-8-ylamino)valeric acid

hydrochloric acid dioxane

→

hydrochloride

title compound

(2S)-2-(4-(N-2-picolylaminomethyl)naphthoylamino)-5-((8R)-5,6,7,8-tetrahydroquinolin-8-ylamino)valeric acid

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe reaction solution was concentrated
2. 2
   SonstigeThe residue was purified by silica gel column chromatography (chloroform/methanol/water=7/3/0.5)
3. 3
   workup.ADDITIONAfter the addition of 1 mol/l hydrochloric acid
4. 4
   Einengenthe residue was concentrated
5. 5
   workup.DISTILLATIONsubjected to azeotropic distillation with methanol

Vorschrift

The compound obtained in Example 54-3 (7.2 mg) was dissolved in methanol (0.15 ml) and 4 mol/l hydrochloric acid/dioxane solution (0.15 ml) was added. After 2 hours, the reaction solution was concentrated. The residue was purified by silica gel column chromatography (chloroform/methanol/water=7/3/0.5). After the addition of 1 mol/l hydrochloric acid, the residue was concentrated and subjected to azeotropic distillation with methanol to obtain hydrochloride of the title compound (6.3 mg) as a white solid.

Quelle