반응 #11436

반응 방정식

Triethylamine

1-(4-aminobutyl)-2-butyl-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-4-amine

4-fluorobenzenesulfonyl chloride

→

N-[4-(4-amino-2-butyl-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-1-yl)butyl]-4-fluorobenzenesulfonamide hydrate

수율 43.0%

용매

dichloromethane

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled in an ice bath
2. 2
   기타the reaction mixture was removed from the ice bath
3. 3
   세척The reaction mixture was washed with water (2×150 mL)
4. 4
   농축concentrated under reduced pressure
5. 5
   기타The resulting residue was recrystallized from methyl acetate
6. 6
   기타dried in an Abderhalden
7. 7
   기타drying apparatus

실험 절차

Triethylamine (0.07 mL, 0.5 mmol) was added to a solution of 1-(4-aminobutyl)-2-butyl-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-4-amine (150 mg, 0.5 mmol) in dichloromethane (150 mL). The reaction mixture was cooled in an ice bath. 4-fluorobenzenesulfonyl chloride (113 mg, 0.5 mmol) was added and the reaction mixture was removed from the ice bath. The reaction mixture was stirred at ambient temperature for 48 hours. The reaction mixture was washed with water (2×150 mL) and then concentrated under reduced pressure. The resulting residue was recrystallized from methyl acetate and then dried in an Abderhalden drying apparatus to provide 50 mg of N-[4-(4-amino-2-butyl-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-1-yl)butyl]-4-fluorobenzenesulfonamide hydrate as a white crystalline solid, m.p. 133.1–133.7° C.

출처