反应详情

2-Methylbenzimidazole-5-carboxylic acid (1.00 g, 5.7 mmol), 2-aminophenol (0.68 g, 6.2 mmol), chloroform (20 mL), triethylamine (0.69 g, 6.8 mmol), and WSC (1.20 g, 6.2 mmol) were stirred overnight at room temperature. After the reaction was complete, water (50 mL) was added to the residue from concentration, and this was extracted with ethyl acetate. After the organic layer was dried over anhydrous sodium sulfate, filtration and concentration gave crystals that were dissolved in dioxane (30 mL), to which methanesulfonic acid (0.48 mL) was added and this was stirred at reflux for 10 hours. After cooling a precipitated solid was filtered off, and washing with THF and drying under reduced pressure at 50° C. yielded the title compound (0.82 g, 42% yield) as a white solid.

1. extractionthis was extracted with ethyl acetate
2. dry with materialAfter the organic layer was dried over anhydrous sodium sulfate, filtration and concentration
3. customgave crystals that
4. additionwas added
5. temperatureat reflux for 10 hours
6. temperatureAfter cooling a precipitated solid
7. filtrationwas filtered off
8. washwashing with THF
9. customdrying under reduced pressure at 50° C.