反应详情

6-Bromomethyl-4-methanesulfonyl-3,4-dihydro-2H-benzo[1,4]oxazine (2.6 g, 8.5 mmol) and tert-butyl piperazine-1-carboxylate (1.58 g, 8.5 mmol) were treated with propan-2-ol (100 mL) followed by N,N-diisopropylethylamine (10.96 g, 85 mmol) and the resulting mixture heated at reflux for 72 h then evaporated to dryness under reduced pressure. The residue was partitioned between ethyl acetate and saturated NaHCO3 aq. and the phases separated. The organic phase was washed with water, saturated brine, dried (MgSO4) and evaporated to dryness under reduced pressure. Chromatography on SiO2, eluting with ethyl acetate in 60°–80° petroleum ether, gave the title compound (2.5 g, 71%) as a brown foam.

1. temperaturethe resulting mixture heated
2. temperatureat reflux for 72 h
3. customthen evaporated to dryness under reduced pressure
4. customThe residue was partitioned between ethyl acetate and saturated NaHCO3 aq.
5. customthe phases separated
6. washThe organic phase was washed with water, saturated brine
7. dry with materialdried (MgSO4)
8. customevaporated to dryness under reduced pressure
9. washChromatography on SiO2, eluting with ethyl acetate in 60°–80° petroleum ether