反应详情

A mixture of methyl 4-(2,4,5-trifluorophenyl)acetoacetate from Example 1 (25.0 g, 102 mmol) and ammonium acetate (38.5 g, 500 mmol) in methanol (250 ml) was stirred at reflux until the starting material totally disappeared (˜4 h). The whole reaction mixture was then concentrated, switched to dichloromethane and filtered. The filtration was washed with water, then brine, then dried over sodium sulfate, filtered and evaporated—ed. The residue oil solidified when hexane was added. The solid was collected by filtration and dried to give 22.4 g of the enamine product (89.6%). 1H NMR (300 MHz, CDCl3) 7.12-7.03 (m, 1H), 6.99-6.90 (m, 1H), 4.56 (s, 1H) 3.65 (s, 3H), 3.40 (s, 2H)

1. temperatureat reflux until the starting material
2. custom(˜4 h)
3. customThe whole reaction mixture
4. concentrationwas then concentrated
5. filtrationfiltered
6. filtrationThe filtration
7. washwas washed with water
8. dry with materialbrine, then dried over sodium sulfate
9. filtrationfiltered
10. customevaporated—ed
11. additionwas added
12. filtrationThe solid was collected by filtration
13. customdried