反应 #11939

反应方程式

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

溶剂

methanol

反应条件

后处理

1. 1
   其他After the completion of the reaction
2. 2
   其他the solvent was removed by distillation
3. 3
   其他The 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
   浓缩concentrated
6. 6
   workup.DISTILLATIONazeotropically distilled with water
7. 7
   洗涤The resulting solid was washed with ether

实验过程

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.

来源