Reaktion #11963

Reaktionsgleichung

compound

(S)-2-(4-(N-Boc-N-2-picolylaminomethyl)benzoylamino)-5-(quinolin-8-ylamino)valeric acid

hydrochloric acid dioxane

→

title compound

(S)-2-(4-(N-2-picolylaminomethyl)benzoylamino)-5-(quinolin-8-ylamino)valeric acid

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe reaction solution was concentrated
2. 2
   workup.DISTILLATIONazeotropically distilled with methanol
3. 3
   SonstigeThe residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5)

Vorschrift

The compound obtained in Example 53-3 (19.0 mg) was dissolved in methanol (0.19 ml) and 4 mol/l hydrochloric acid/dioxane (0.19 ml) was added. After 2.5 hours, the reaction solution was concentrated and azeotropically distilled with methanol. The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5). The obtained title compound was dissolved in methanol. Activated carbon (4 mg) was added to the solution, followed by filtration and concentration. After the addition of 1 mol/l hydrochloric acid and a small amount of methanol, the residue was concentrated and dried under reduced pressure to obtain hydrochloride of the title compound (17.9 mg) as a yellow solid.

Quelle