반응 #528443

반응 방정식

5-(4-[2-(4-methylphenyl)benzoylamino]-benzoyl}-1,3,4,5-tetrahydro-1,5-benzodiazepine-2(2H)thione

3-dimethylaminopropyl chloride hydrochloride

potassium carbonate

sodium iodide

→

2-[3-(dimethylamino)propylthio]-5-{4-[2-(4-methylphenyl)benzoylamino]benzoyl}-4,5-dihydro-3H-1,5benzodiazepine

수율 37.1%

용매

acetone

반응 조건

후처리

1. 1
   여과The mixture was filtered
2. 2
   기타the filtrate was evaporated
3. 3
   기타The residue was purified by column chromatography (SiO2 30 g, 5% methanol in chloroform)

실험 절차

A solution of 5-(4-[2-(4-methylphenyl)benzoylamino]-benzoyl}-1,3,4,5-tetrahydro-1,5-benzodiazepine-2(2H)thione (460 mg), 3-dimethylaminopropyl chloride hydrochloride (740 mg), potassium carbonate (1.29 g) and sodium iodide (catalytic amount) in acetone (40 ml) was stirred for 19 hours at 60° C. The mixture was filtered and the filtrate was evaporated. The residue was purified by column chromatography (SiO2 30 g, 5% methanol in chloroform) to give 2-[3-(dimethylamino)propylthio]-5-{4-[2-(4-methylphenyl)benzoylamino]benzoyl}-4,5-dihydro-3H-1,5benzodiazepine (200 mg).

출처