反应详情

温度

140 °C

A mixture of 2-chloro-6-nitro-quinoline (2.0 g, 9.6 mmol) in 1-methyl-2-pyrrolidone (5 mL) with the above described rac-4-ethoxy-2,3-dihydro-benzofuran-3-ylamine (3.78 g, ca. 10 mmol, max. 50% purity) and N-ethyldiisopropylamine (2.45 mL, 14.4 mmol) was stirred at 140° C. for 2 h. Cooled to 23° C., poured onto water and extracted twice with ethyl acetate, dried over Na2SO4 and evaporated totally to give a crude product which was purified by silica gel column chromatography with heptane/dichloromethane followed by trituration with diethyl ether to give the title compound as a yellow solid (0.60 g, 18%); MS: m/e=352.4 (M+H+).

1. temperatureCooled to 23° C.
2. additionpoured onto water
3. extractionextracted twice with ethyl acetate
4. dry with materialdried over Na2SO4
5. customevaporated totally
6. customto give a crude product which
7. customwas purified by silica gel column chromatography with heptane/dichloromethane