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温度

0 °C

A mixture of methyl 4-acetylbenzoate (25 g, 140 mmol) and N,N-dimethylformamide dimethyl acetal (100 mL) was heated to reflux for 2 days, diluted with MeOH (100 mL) and cooled to 0° C. The precipitate was collected by filtration and washed with MeOH to give (E)-methyl 4-(3-(dimethylamino)acryloyl)benzoate as a brown solid (27.65 g, 84% yield). MS (ES+) m/z: 234 (M+H); LC retention time: 2.91 min (analytical HPLC Method A).

1. temperaturewas heated
2. temperatureto reflux for 2 days
3. filtrationThe precipitate was collected by filtration
4. washwashed with MeOH