반응 #1783406

반응 방정식

ammonium chloride

4-(cyclohexylamino)-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid

1-hydroxybenzotriazole

1-(3-dimethylaminopropyl)-3-ethylcarbodiimide

→

4-(cyclohexylamino)-1H-pyrrolo[2,3-b]pyridine-5-carboxamide

수율 60.2%

용매

chloroform

water

N,N-dimethylformamide

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture was stirred at ambient temperature for 18 hours
2. 2
   추출the mixture was extracted with chloroform
3. 3
   건조The extract was dried over MgSO4
4. 4
   여과filtrated
5. 5
   기타evaporated in vacuo
6. 6
   기타The residue was purified by column chromatography on silica gel with chloroform and methanol (100:0 to 90:10)

실험 절차

To a solution of 4-(cyclohexylamino)-1H-pyrrolo[2,3-b]pyridine-5-carboxylic acid (5.0 mg) in N,N-dimethylformamide (0.1 mL) were added 1-hydroxybenzotriazole (3.9 mg) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (4.5 mg). The mixture was stirred at 60° C. for 30 minutes. To the solution was added ammonium chloride and the mixture was stirred at ambient temperature for 18 hours. To the solution were added water and chloroform and the mixture was extracted with chloroform. The extract was dried over MgSO4, filtrated and evaporated in vacuo. The residue was purified by column chromatography on silica gel with chloroform and methanol (100:0 to 90:10) to give 4-(cyclohexylamino)-1H-pyrrolo[2,3-b]pyridine-5-carboxamide (3 mg) as a white powder.

출처