反应详情

温度

-78 °C

1H-benzo[d]imidazole-5-carboxylic acid (10 mmol, 1 eq.) was dissolved in 30 mL THF and cooled down to −78° C. 20 mL 1 M solution of lithium aluminium hydride (20 mmol, 2 eq.) were added slowly. After stirring at ambient temperature for 10 hours the reaction was quenched with methanol. The solvent was removed, 50 mL aqueous solution of sodium hydrogen carbonate was added and extracted with 50 mL ethyl acetat three times. The combined organic layers were dried over sodium sulfate, filtrated and the solvent was removed under reduced pressure. The product was purified by means of flash-chromatography using silica gel and a ethyl acetate/MeOH-gradient.

1. customwas quenched with methanol
2. customThe solvent was removed
3. addition50 mL aqueous solution of sodium hydrogen carbonate was added
4. extractionextracted with 50 mL ethyl acetat three times
5. dry with materialThe combined organic layers were dried over sodium sulfate
6. filtrationfiltrated
7. customthe solvent was removed under reduced pressure
8. customThe product was purified by means of flash-chromatography