反应详情

温度

61.5 °C

The methyl 4-(2,4,5-trifluorophenyl)acetoacetate (350.0 gm, 1.42 mol) (21) and ammonium acetate (6.0 eq, 657.0 gm) were charged in methanol (5.0 vol, 1.75 Ltr) and the solution was refluxed for 5-6 hours at 60-63° C. After 5-6 hours refluxing, the methanol was distilled out completely to give a pale yellow coloured residue. The pale yellow coloured residue was further stirred with ethyl acetate (20.0 vol, 7.0 Ltr) at 25-30° C. The precipitated ammonium acetate was filtered and the ethyl acetate was distilled out completely to give a pale yellow product. The product was further stirred with hexane (10.0 vol, 3.5 Ltr) at 25-30° C. for 1 hour, filtered and dried under reduced pressure at 45-50° C. for 4-5 hours.

1. temperatureAfter 5-6 hours refluxing
2. distillationthe methanol was distilled out completely
3. customto give a pale yellow coloured residue
4. filtrationThe precipitated ammonium acetate was filtered
5. distillationthe ethyl acetate was distilled out completely
6. customto give a pale yellow product
7. filtrationfiltered
8. customdried under reduced pressure at 45-50° C. for 4-5 hours