반응 #833560

반응 방정식

sodium thiosulphate

1-bromo-2-butyne

dimethyl 2-bromo-1H-imidazole-4,5-dicarboxylate

potassium carbonate

→

dimethyl 2-bromo-1-(but-2-ynyl)-1H-imidazole-4,5-dicarboxylate

용매

dimethylformamide

반응 조건

후처리

1. 1
   기타The organic phase is separated off
2. 2
   추출the aqueous phase is extracted three times with ethyl acetate
3. 3
   건조The combined organic phases are dried over sodium sulphate
4. 4
   기타the solvent is removed
5. 5
   기타the residue is chromatographed over silica gel (cyclohexane/ethyl acetate 4:1>1:1)

실험 절차

3.06 g 1-bromo-2-butyne are added dropwise to a mixture of 6.00 g of dimethyl 2-bromo-1H-imidazole-4,5-dicarboxylate and 3.80 g of potassium carbonate in 40 ml of dimethylformamide. The mixture is stirred for 12 h at ambient temperature and then added to an aqueous saturated solution of sodium thiosulphate. The organic phase is separated off and the aqueous phase is extracted three times with ethyl acetate. The combined organic phases are dried over sodium sulphate, the solvent is removed and the residue is chromatographed over silica gel (cyclohexane/ethyl acetate 4:1>1:1).

출처