반응 #347448

반응 방정식

2-phenyl-imidazole

sodium hydride

N-(4-bromobutyl)-phthalimide

→

expected product

수율 17.2%

4-(2-phenyl-1H-imidazol-1-yl)-butylamine

수율 17.2%

용매

dimethylformamide

dimethylformamide

dimethylformamide

반응 조건

후처리

1. 1
   추출extraction
2. 2
   기타by drying
3. 3
   기타The solvent has evaporated
4. 4
   기타the residue was chromatographed on silica (eluant: ethyl acetate-methylethylamine 95-5)
5. 5
   온도chilled
6. 6
   기타the crystals were separated out and
7. 7
   기타dried

실험 절차

4.32 g of 2-phenyl-imidazole in solution in 25 ml of dimethylformamide were added over 75 minutes at ambient temperature to 1.73 g of sodium hydride in 5 ml of dimethylformamide and then, 10.97 g of N-(4-bromobutyl)-phthalimide in 33 ml of dimethylformamide were added. The mixture was stirred for 48 hours at ambient temperature and extraction was carried out with ethyl acetate, followed by drying. The solvent has evaporated and the residue was chromatographed on silica (eluant: ethyl acetate-methylethylamine 95-5). The residue was taken up in ether, chilled and the crystals were separated out and dried to obtain 1.11 g of the expected product melting at 82°-84° C.

출처