反应详情

温度

17.5 °C

75.0 g (0.36 moles) of N-(5-acetyl-2-fluorophenyl)-N-methyl-acetamide (VI) were dissolved in 96.3 mL (86.4 g, 0.72 moles) of NNDMF-DMA. The resulting solution was refluxed for 8 hours. At the temperature of 80° C., 400 mL of toluene were added, and then, at the same temperature, 400 mL of n-heptane were slowly added. The resulting solution was slowly cooled to 15-20° C. The white-yellowish solid obtained by recrystallization was filtered off, washed with 263 mL of toluene:n-heptane (1:1), and then dried under vacuum at 40° C. A white-yellowish solid (84.1 g, 91.7% yield) with a melting point=131-132° C. was obtained.

1. temperatureThe resulting solution was refluxed for 8 hours
2. customThe white-yellowish solid obtained by recrystallization
3. filtrationwas filtered off
4. washwashed with 263 mL of toluene:n-heptane (1:1)
5. customdried under vacuum at 40° C