反応 #1518673
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09265773B2
反応条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: The mixture of 1-(5-bromo-2-methoxyphenyl)ethanone (10 g, 43.6 mmol), phenylhydrazine (7.07 g, 65.5 mmol) was stirred in PPA (50 mL) at 110° C. for 2 hours. The reaction mixture was added to water and basified to pH=7, then extracted with ethyl acetate and washed with brine, dried over Na2SO4. After concentrated, the resulting residue was purified using column chromatography to provide the product of 2-(5-bromo-2-methoxyphenyl)-1H-indole (10 g, yield: 71%). 1H-NMR (CDCl3, 400 MHz) δ 9.57 (s, 1H), 7.93 (d, J=2.4 Hz, 1H), 7.63 (d, J=8.0 Hz, 1H), 7.34˜7.42 (m, 2H), 7.09˜7.21 (m, 2H), 6.90 (d, J=8.8 Hz, 1H), 4.00 (s, 3H). MS (M+H)+: 302/304. extracted with ethyl acetate washed with brine dried over Na2SO4 After concentrated the resulting residue was purified
ソース ID: ord-f68f82b705ee4f0f80cf1dae345c3ba3