Reaktion #11939

Reaktionsgleichung

compound

(S)-2-(4-(N-Boc-2-picolylaminoethyl)benzoyl)amino-5-(2-picolylamino)valeric acid

hydrochloric acid dioxane

→

hydrochloride

title compound

(S)-2-(4-(2-(N-2-picolylamino)ethyl)benzoylamino)-5-(N-2-picolylamino)valeric acid

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter the completion of the reaction
2. 2
   Sonstigethe solvent was removed by distillation
3. 3
   SonstigeThe residue was purified by silica gel column chromatography (0.5 g, chloroform/methanol/water=7/3/0.5)
4. 4
   workup.ADDITIONThe obtained product was added with 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 10-1 (13.9 mg) was dissolved in methanol (0.28 ml) and 4 mol/l hydrochloric acid/dioxane solution (0.28 ml) was added to the solution. The mixture was stirred for 75 minutes at room temperature. After the completion of the reaction, the solvent was removed by distillation. The residue was purified by silica gel column chromatography (0.5 g, chloroform/methanol/water=7/3/0.5). The obtained product was added with 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 (13.8 mg) as a white solid.

Quelle