تفاعل #11939

معادلة التفاعل

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

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter the completion of the reaction
2. 2
   أخرىthe solvent was removed by distillation
3. 3
   أخرىThe 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
   تركيزconcentrated
6. 6
   workup.DISTILLATIONazeotropically distilled with water
7. 7
   غسيلThe resulting solid was washed with ether

الإجراء التجريبي

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.

المصدر