反应详情

温度

0 °C

21 g (520 mmol) of 60% sodium hydride are suspended in 700 ml of anhydrous DMF under an inert atmosphere, and the mixture is cooled to 0° C. 40.5 g (260 mmol) of 2,2,2-trifluoro-N-isopropylacetamide are slowly added portionwise. After 15 minutes, 62 ml (520 mmol) of 1,4-dibromobutane are added. The reaction medium is then heated at 60° C. for 3 hours, and then cooled to room temperature, poured into 1 L of water and extracted with ethyl acetate. The organic phase is washed with water and dried, and the residue obtained is purified by distillation. A colorless oil is obtained (m=0.18 g, yield=24%).

1. temperatureThe reaction medium is then heated at 60° C. for 3 hours
2. temperaturecooled to room temperature
3. extractionextracted with ethyl acetate
4. washThe organic phase is washed with water
5. customdried
6. customthe residue obtained
7. distillationis purified by distillation
8. customA colorless oil is obtained (m=0.18 g, yield=24%)