반응 #11939

반응 방정식

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

용매

methanol

반응 조건

후처리

1. 1
   기타After the completion of the reaction
2. 2
   기타the solvent was removed by distillation
3. 3
   기타The 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
   농축concentrated
6. 6
   workup.DISTILLATIONazeotropically distilled with water
7. 7
   세척The resulting solid was washed with ether

실험 절차

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.

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