反应 #11945

反应方程式

compound

(2S)-2-(2-(N-Boc-N-2-picolylaminomethyl)pyridin-5-ylcarbonyl)amino-5-(5,6,7,8-tetrahydroquinolin-8-yl)aminovaleric acid

hydrochloric acid dioxane

→

hydrochloride

title compound

(2S)-2-(2-(N-2-picolylaminomethyl)pyridin-5-ylcarbonyl)amino-5-((5,6,7,8-tetrahydroquinolin-8-yl)amino)valeric acid

溶剂

methanol

反应条件

后处理

1. 1
   其他After 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 (1 g, chloroform/methanol/water=7/3/0.5)
4. 4
   workup.ADDITIONThe obtained product was added with an aqueous solution of hydrochloric acid
5. 5
   workup.DISTILLATIONazeotropically distilled with water
6. 6
   洗涤The resulting solid was washed with ether

实验过程

The compound obtained in Example 12-5 (26.8 mg) was dissolved in methanol (0.5 ml), and 4 mol/l hydrochloric acid/dioxane solution (0.5 ml) was added. The mixture was stirred for 4.5 hours at room temperature. After the reaction, the solvent was removed by distillation. The residue was purified by silica gel column chromatography (1 g, chloroform/methanol/water=7/3/0.5). The obtained product was added with an aqueous solution of hydrochloric acid and concebtrated, and then azeotropically distilled with water. The resulting solid was washed with ether to obtain a hydrochloride of the title compound (25.8 mg) as a white solid.

来源