反应详情

To a solution of 3-amino-4-hydroxymethyl-6-methyl-thieno[2,3-b]pyridine-2-carboxamide (100 mg, 0.42 mmol) in acetic acid (2 mL) was added benzaldehyde (53 mg, 0.50 mmol) and the mixture was heated to reflux for 16 h. After cooling to room temperature, water (2 mL) and ethyl acetate (2 mL) were added to it. The reaction was further extracted with ethyl acetate (2 mL×3). The combined organic layers were washed with brine, dried over Na2SO4 and evaporated under reduced pressure. The residue was purified by preparative HPLC to give the title compound, 4-hydroxymethyl-2-methyl-6-phenyl-6,7-dihydro-5H-9-thia-1,5,7-triaza-fluoren-8-one (16 mg, 12%).

1. temperaturethe mixture was heated
2. temperatureto reflux for 16 h
3. extractionThe reaction was further extracted with ethyl acetate (2 mL×3)
4. washThe combined organic layers were washed with brine
5. dry with materialdried over Na2SO4
6. customevaporated under reduced pressure
7. customThe residue was purified by preparative HPLC