反应详情

2-Chloro-1-fluoro-4-nitrobenzene (10 g, 57 mmol) and 1-acetylpiperazine (14.6 g, 114 mmol) were heated neat at 55° C. for 1 h. Then the reaction mixture was allowed to cool down to room temperature. The viscous orange solution was diluted with EtOAc and water. The organics were washed with water (3 times), brine, dried and evaporation of the solvent gave an orange oil which was triturated with isohexane. After evaporation of solvent the title compound was obtained as a yellow solid which was dried overnight in vac oven at 50° C. (15.68 g, 97%). It was used without further purification. NMR (400 MHz) 2.03 (d, 3H), 3.18 (dt, 4H), 3.62 (m, 4H), 7.30 (d, 1H), 8.17 (dd, 1H), 8.26 (d, 1H); m/z 284-286.

1. washThe organics were washed with water (3 times), brine
2. customdried
3. customevaporation of the solvent
4. customgave an orange oil which
5. customwas triturated with isohexane
6. customAfter evaporation of solvent the title compound
7. customwas obtained as a yellow solid which
8. customwas dried overnight in vac oven at 50° C. (15.68 g, 97%)
9. customIt was used without further purification