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温度

0 °C

(Cyano)thioacetamide (2 g, 19.97 mmol) was stirred in excess THF (40 mL) under nitrogen atmosphere. The solution was cooled to 0° C. and the solution of 3-bromopyruvic acid (3.33 g, 19.97 mmol) dissolved in 5 mL THF was added dropwise. The mixture was refluxed for 3 h. Solvent was evaporated and the crude product was purified by flash chromatography (silica, eluent: 0-40% DCM-10% MeOH/DCM mixture) to yield 1.615 g of the title compound. 1H NMR (400 MHz; CDCl3): δ 4.20 (s, 2H), 8.33 (s, 1H).

1. additionwas added dropwise
2. temperatureThe mixture was refluxed for 3 h
3. customSolvent was evaporated
4. customthe crude product was purified by flash chromatography (silica, eluent: 0-40% DCM-10% MeOH/DCM mixture)