反应详情

温度

100 °C

7.2 g (39.3 mmol) 1H-Imidazol-2-ylamine sulfate are dissolved in 45 mL DMF. 10 g (39.3 mmol) diethyl (4-fluorophenyl)malonate is added. After dropwise addition of 17.6 mL (118 mmol) 1,8-diazabicyclo[5.4.0]undec-7-ene the reaction mixture is stirred at 100° C. over night. The DMF has been removed and the darkbrown oily residue treated with 150 mL water (complete dissolution). 2M HCl (60 mL) is added at room temperature until a pH of 1. After stirring for 1 h at ice bath cooling the formed crystals are collected by filtration to yield the product (5.78 g=53.9%), which is used without further purification. Another crop of 0.48 g (4.5%) is obtained by treating the solid residue in the flask with water and 2M HCl. After stirring for one hour the crystals are collected.

1. customThe DMF has been removed
2. additionthe darkbrown oily residue treated with 150 mL water (complete dissolution)
3. addition2M HCl (60 mL) is added at room temperature until a pH of 1
4. stirringAfter stirring for 1 h at ice bath
5. temperaturecooling the formed crystals
6. filtrationare collected by filtration
7. customto yield the product (5.78 g=53.9%), which
8. customis used without further purification
9. customAnother crop of 0.48 g (4.5%) is obtained
10. stirringAfter stirring for one hour the crystals
11. customare collected