反应详情

温度

70 °C

Ethyl N-(2-methoxy-6-methylquinoxalin-3-yl)carbamate (26 mg, 0.10 mmol) and 1-phenylpiperazine (24 mg, 0.15 mmol) were dissolved in tetrahydrofuran (2 ml) at room temperature and thereto DBU (23 mg, 0.15 mmol) was added. The resulting mixture was stirred at 70° C. for 7 hours and concentrated under the reduced pressure to remove the solvent, and purified by SiO2 column chromatography. Extraction of the residue with a n-hexane:ethyl acetate (2:1) mixture and concentration gave 34 mg of the titled compound (yield, 90%). 1H NMR (300 MHz, CDCl3): δ 2.42-2.48 (m, 3H), 3.22-3.30 (m, 4H), 3.77 (s, 3H), 4.12 (s, 4H), 6.90-7.12 (m, 4H), 7.25-7.32 (m, 3H), 7.48-7.65 (m, 2H).

1. concentrationconcentrated under the reduced pressure
2. customto remove the solvent
3. custompurified by SiO2 column chromatography
4. extractionExtraction of the residue
5. concentrationwith a n-hexane:ethyl acetate (2:1) mixture and concentration