反应详情

温度

55 °C

0.8 g (1.86 mmol) of 2-(4-cyanophenylaminomethyl)-1-methyl-5-[1-amino-1-(pyrrolidin-1-yl-carbonyl)-ethyl]-benzimidazole and 1.65 g ((5.5 mmol) of tert.butyl 2,4-dibromobutyrate are dissolved in 5 ml of ethanol, mixed with 0.2 g (1.86 mmol) of sodium carbonate and stirred under nitrogen for 30 hours at 55° C. After cooling, the white precipitate is filtered off and washed with ethanol. The filtrate is concentrated by evaporation, the residue is chromatographed on silica gel, eluting with ethyl acetate and ethyl acetate/ethanol/ammonia (20:1:0.01). The desired fractions are combined and concentrated by evaporation.

1. temperatureAfter cooling
2. filtrationthe white precipitate is filtered off
3. washwashed with ethanol
4. concentrationThe filtrate is concentrated by evaporation
5. customthe residue is chromatographed on silica gel
6. washeluting with ethyl acetate and ethyl acetate/ethanol/ammonia (20:1:0.01)
7. concentrationconcentrated by evaporation