反应 #833560

反应方程式

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

溶剂

dimethylformamide

反应条件

后处理

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

实验过程

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).

来源