反应详情

A solution of 116 g (0.41 mol) of methyl 2-azido-3-(2-bromophenyl)prop-2-enoate in 1.5 l of toluene is added dropwise over 4 h, with mechanical stirring, to a solution of 2 l of toluene heated to reflux and reflux is maintained for an additional 1 h. The solvent is evaporated under reduced pressure and the residue is taken up in 2 l of cyclohexane. The precipitate is collected by filtration, washed with toluene and dried under reduced pressure 37.85 g (149 mmol) of product are isolated. The mother liquors are concentrated under reduced pressure and the residue is purified by chromatography on a column of silica gel. 12.2 g (48 mmol) of additional product are isolated.

1. temperatureheated
2. temperatureto reflux
3. temperaturereflux
4. temperatureis maintained for an additional 1 h
5. customThe solvent is evaporated under reduced pressure
6. filtrationThe precipitate is collected by filtration
7. washwashed with toluene
8. customare isolated
9. concentrationThe mother liquors are concentrated under reduced pressure
10. customthe residue is purified by chromatography on a column of silica gel