反应详情

Into a 25-mL round-bottom flask placed ethyl 2-amino-5-methylthiophene-3-carboxylate (500 mg, 2.70 mmol, 1.00 equiv) in 10 mL of formamide was stirred for 8 h at 180° C. in an oil bath. After completion of the reaction, the reaction mixture was cooled down to room temperature and then quenched with water/ice, extracted with 3×50 mL of ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was purified on a silica gel column with ethyl acetate/petroleum ether (2:1) to provide the resulted 6-methylthieno[2,3-d]pyrimidin-4-ol (114 mg, 25%) as a yellow solid. MS (ES, m/z): 167 [M+H+].

1. customInto a 25-mL round-bottom flask placed
2. customAfter completion of the reaction
3. customquenched with water/ice
4. extractionextracted with 3×50 mL of ethyl acetate
5. washThe combined organic layers were washed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationconcentrated under vacuum
8. customThe residue was purified on a silica gel column with ethyl acetate/petroleum ether (2:1)