反应详情

温度

23 °C

A mixture of the above described 2-chloro-N-[2-((R)-indan-1-ylamino)-4H-benzo[d][1,3]oxazin-6-yl]-acetamide (800 mg, 2.248 mmol) and 1-methylpiperazine (5 ml, 45 mmol) was stirred at 23° C. for 18 h. Diluted with ethyl acetate, washed with sat. sodium hydrogen carbonate-solution, dried the organic layer over sodium sulfate. Filtration and removal of the solvent in vacuum left a crude product which was purified by silica gel column chromatography with ethyl acetate to ethyl acetate +10% methanol-ammonium hydroxide (10:1) and trituration with diethyl ether to give the title compound as a white foam (320 mg, 34%), MS (ISP) m/e=420.2 [(M+H)+].

1. additionA mixture of the
2. washwashed with sat. sodium hydrogen carbonate-solution
3. dry with materialdried the organic layer over sodium sulfate
4. filtrationFiltration and removal of the solvent in vacuum
5. waitleft a crude product which
6. customwas purified by silica gel column chromatography with ethyl acetate to ethyl acetate +10% methanol-ammonium hydroxide (10:1) and trituration with diethyl ether