反应详情

温度

20 °C

To a solution containing 0.93 g 3-fluoro-4-methylsulfonylbenzaldehyde, 0.05 ml piperidine and 0.02 ml formic acid in 20 ml DMF was added 1.04 ml 2,4-pentanedione with stirring at 20° C. The solution was stirred overnight at 20° C. and poured into water. The product was extracted with ethyl acetate and washed with water and evaporated to dryness in vacuo. The residue was crystallized from methanol, yield 0.48 g (30%), mp. 140-143° C. 1H-NMR (DMSO-d6, 400 MHz): 2.28 (s, 3 H, CH3), 2.50 (s, 3 H, CH3), 3.36 (s, 3 H, CH3), 7.47 (m, 1 H, Ar), 7.93 (m, 2 H, Ar), 7.76 (s, 1 H, CH).

1. stirringThe solution was stirred overnight at 20° C.
2. extractionThe product was extracted with ethyl acetate
3. washwashed with water
4. customevaporated to dryness in vacuo
5. customThe residue was crystallized from methanol, yield 0.48 g (30%), mp. 140-143° C