反应详情

温度

60 °C

A 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer and nitrogen inlet was charged with DMF (20 mL), 3-nitro-1H-pyrazole (1.00 g, 8.84 mmol), N-tert-butoxycarbonyl-3-iodoazetidine (3.00 g, 10.6 mmol) and potassium carbonate (2.45 g, 17.7 mmol), and the reaction mixture was stirred at 60° C. for 16 h. After this time the reaction was concentrated to dryness under reduced pressure, and the resulting residue was mixed with methylene chloride (15 mL) and water (15 mL). The aqueous layer was separated and extracted with methylene chloride (2×15 mL). The combined organic extracts were dried over sodium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography to afford an 80% yield (1.92 g) of 105a as a yellow oil: 1H NMR (300 MHz, CDCl3) δ 7.64 (d, 1H, J=2.4 Hz), 6.97 (d, 1H, J=2.4 Hz), 5.13 (m, 1H), 4.44 (m, 2H), 4.33 (m, 2H), 1.47 (s, 9H).

1. customA 100-mL single-neck round-bottomed flask equipped with a magnetic stirrer and nitrogen inlet
2. concentrationAfter this time the reaction was concentrated to dryness under reduced pressure
3. additionthe resulting residue was mixed with methylene chloride (15 mL) and water (15 mL)
4. customThe aqueous layer was separated
5. extractionextracted with methylene chloride (2×15 mL)
6. dry with materialThe combined organic extracts were dried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by column chromatography