反応 #833560

反応方程式

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

溶媒

dimethylformamide

反応条件

後処理

1. 1
   その他The organic phase is separated off
2. 2
   抽出the aqueous phase is extracted three times with ethyl acetate
3. 3
   乾燥The combined organic phases are dried over sodium sulphate
4. 4
   その他the solvent is removed
5. 5
   その他the residue is chromatographed over silica gel (cyclohexane/ethyl acetate 4:1>1:1)

実験手順

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).

出典