反应详情

温度

101.5 °C

Potassium carbonate (3.3 g, 24 mmol) and 1-methylpiperazine (2.8 g, 29 mmol) were dissolved in 16 mL of water and then 4-fluorobenzaldehyde (2.0 g, 16 mmol) was added. The mixture was heated at reflux (100-103° C.) under a nitrogen atmosphere for 21 hours when HPLC showed that the reaction was complete. The solution was cooled to 20-25° C. and then extracted with methylene chloride (2×30 mL). The methylene chloride extracts were combined, washed with water (2×30 mL), and then concentrated at reduced pressure to a yellow oil (3.1 g, 96% yield). The crude solid was triturated with hexanes to afford crystals. mp 60.5-62.0° C. 1H NMR (CDCl3) δ 9.77 (s, 1H), 7.74 (d, J=10 Hz, 2H), 6.91 (d, J=10 Hz, 2H), 3.40 (m, 4H), 2.53 (m, 4H), and 2.34 (s, 3H).

1. temperatureThe mixture was heated
2. temperatureThe solution was cooled to 20-25° C.
3. extractionextracted with methylene chloride (2×30 mL)
4. washwashed with water (2×30 mL)