반응 #156238

반응 방정식

2-Phenyl-1H-benzimidazole

potassium carbonate

1-ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione

hydrogen chloride ethanol

→

title compound

1-ethyl-3,3,5-trimethyl-7-[3-(2-phenyl-benzoimidazol-1-yl)propoxy]-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione hydrochloride

용매

DMF

isopropyl alcohol

반응 조건

후처리

1. 1
   기타the generated insoluble matter was separated
2. 2
   workup.DISSOLUTIONThe insoluble matter was dissolved in ethyl acetate
3. 3
   건조The liquid was dried over sodium sulfate and condensed under reduced pressure
4. 4
   기타The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:3)
5. 5
   기타condensed under reduced pressure
6. 6
   기타condensed under reduced pressure
7. 7
   기타The generated insoluble matter was separated by filtration
8. 8
   기타dried

실험 절차

2-Phenyl-1H-benzimidazole (0.2 g) and potassium carbonate (0.29 g) were added to a DMF solution (5 ml) of 1-ethyl-7-(3-iodopropoxy)-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (0.49 g). The mixture was stirred at 60° C. for 7 hours. The reaction mixture was poured to ice water (50 ml), and the generated insoluble matter was separated. The insoluble matter was dissolved in ethyl acetate. The liquid was dried over sodium sulfate and condensed under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:3). The purified product was condensed under reduced pressure. A 1N-hydrogen chloride ethanol solution (1.0 ml) was added to an isopropyl alcohol solution of the residue. The mixture was condensed under reduced pressure. Ether was added to the residue. The generated insoluble matter was separated by filtration and dried to give the title compound (0.32 g) as a white powder.

출처