反应详情

A solution of ethyl 2-(2-fluoro-5-iodobenzoyl)-3-(2-morpholinoethylamino)acrylate (Intermediate 23, 358 mg, 0.75 mmol) and potassium carbonate (208 mg, 1.50 mmol) in DMF (7 mL) was heated to 100° C. for 4 h. The reaction mixture was cooled to room temperature, filtered, and concentrated under reduced pressure. The solid that formed was placed under high vacuum overnight (328 mg) to yield the desired product. MS (ESP): 457 (M+H+) for C18H21IN2O4; NMR: 1.28 (t, J=7 Hz, 3H), 2.43 (m, 4H), 2.61 (m, 2H), 3.50 (m, 4H), 4.22 (q, J=7 Hz, 2H), 4.46 (m, 2H), 7.67 (d, J=9 Hz, 1H), 8.05 (m, 1H), 8.50 (s, 1H), 8.63 (s, 1H).

1. filtrationfiltered
2. concentrationconcentrated under reduced pressure
3. customThe solid that formed
4. customwas placed under high vacuum overnight (328 mg)