反应详情

温度

130 °C

Part B. A mixture of 3-dimethylamino-1-(4-fluoro-phenyl)-propan-1-one (641.9 mg, 3.10 mmol) and 3-carbamimidoyl-benzoic acid tert-butyl ester (426.1 mg, 1.91 mmol) in anhydrous acetic acid (8 mL) is heated to 130° C. at 300 W, 250 psi in a microwave reactor for 30 min. A white solid is precipitated by addition of 1 N HCl, and collected by filtration, followed by washing with water and hexanes. The obtained solid is further purified by flash column chromatography, eluting with methanol/methylene chloride (1:40) to afford the title product (114.1 mg, 12.0% yield), m.p. 272-275° C. 1H NMR (300 MHz, DMSO-d6): δ 8.50 (2H, d, J=8.0 Hz), 8.06 (2H, d, J=8.0 Hz), 7.85 (2H, m), 8.13 (2H, m), 7.38 (2H, m), 2.40 (3H, s). MS (ES+): m/e 309.34.

1. customA white solid is precipitated by addition of 1 N HCl
2. filtrationcollected by filtration
3. washby washing with water and hexanes
4. customThe obtained solid is further purified by flash column chromatography
5. washeluting with methanol/methylene chloride (1:40)