反应详情

温度

95 °C

After dissolving 15.5 g of 5-fluoro-2-nitrotoluene (0.1 mol) and 12.8 g of 3-acetamido-pyrrolidine (0.1 mol) in 75 ml of NMP, 15.8 g of potassium carbonate (0.12 mol) are added under a nitrogen atmosphere and the mixture is heated at 95° C. for 20 h. The reaction medium is allowed to cool and is then poured into 600 ml of saturated aqueous sodium chloride solution. The yellow precipitate formed is filtered off, washed with 15% NaCl solution until a pH equal to 7 is obtained for the washing waters, and washed with petroleum ether and then dried in a vacuum oven over P2O5. 25.7 g (98%) of N-[1-(3-methyl-4-nitrophenyl)pyrrolidin-3-yl]acetamide are thus obtained in the form of a yellow solid.

1. additionare added under a nitrogen atmosphere
2. temperatureto cool
3. customThe yellow precipitate formed
4. filtrationis filtered off
5. washwashed with 15% NaCl solution until a pH equal to 7
6. customis obtained for the washing waters
7. washwashed with petroleum ether
8. dry with materialdried in a vacuum oven over P2O5