反应详情

温度

110 °C

A mixture of 90 mg (0.347 mmol) of 2-chloro-7-(2,5-dimethyl-1H-pyrrol-1-yl)-1-methyl-1H-benzimidazole and 225 mg (1.04 mmol) of 4-bromo-2-methoxy-6-methylaniline was stirred at 110° C. for 15 hours. After cooling, the reaction mixture was neutralized by saturated aqueous sodium hydrogen carbonate and extracted with ethyl acetate (X2). The combined organic layer was washed with brine (X1), dried over sodium sulfate and concentrated in vacuo. The residue was purified by silica gel column chromatography eluting with a 60-90% ethylacetate/n-hexane gradient mixture. The desired fractions were collected and evaporated in vacuo, the residual solids were washed with diethyl ether to give 53.4 mg (35%) of the title compound.

1. temperatureAfter cooling
2. extractionextracted with ethyl acetate (X2)
3. washThe combined organic layer was washed with brine (X1)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo
6. customThe residue was purified by silica gel column chromatography
7. washeluting with a 60-90% ethylacetate/n-hexane gradient mixture
8. customThe desired fractions were collected
9. customevaporated in vacuo
10. washthe residual solids were washed with diethyl ether