反应详情

温度

75 °C

A mixture of 1-{4-[(6-bromohexyl)oxy]but-1-ynyl}-3-nitrobenzene (4.18 g), sodium acetate (9.68 g), tetrabutylammonium bromide (384 mg) in DMF (15 ml) and water (10 ml) was heated to 75° C. for 6 h. The mixture was then allowed to cool to 20° C. and then extracted with Et2O. The organic solution was concentrated and purified by chromatography on a Biotage (40 g) eluting with Et2O-petroleum ether(1:19 increasing to 1:1) to give the title compound (2.973 g). LCMS RT=3.84 min.

1. temperatureto cool to 20° C.
2. extractionextracted with Et2O
3. concentrationThe organic solution was concentrated
4. custompurified by chromatography on a Biotage (40 g)
5. washeluting with Et2O-petroleum ether(1:19 increasing to 1:1)