反应详情

温度

-78 °C

5-Hydroxy-2-nitrobenzaldehyde (6.0 g) is dissolved in dry tetrahyrofuran (90 ml) and thereto is added dropwise vinylmagnesium bromide (2.3 equivalents) with stirring at -78° C. The temperature of the reaction mixture is raised gradually. After completion of the reaction, 1N HCl is added to the reaction mixture, and the mixture is extracted with ethyl acetate, and the organic layer is separated, washed with an aqueous saturated saline solution, dried over sodium sulfate, and then distilled off the solvent. The residue is purified with a silica gel column chromatography to give 1-(5'-hydroxy-2'-nitrophenyl)-2-propen-1-ol (5.09 g) as yellowish brown powders.

1. temperatureThe temperature of the reaction mixture is raised gradually
2. additionis added to the reaction mixture
3. extractionthe mixture is extracted with ethyl acetate
4. customthe organic layer is separated
5. washwashed with an aqueous saturated saline solution
6. dry with materialdried over sodium sulfate
7. distillationdistilled off the solvent
8. customThe residue is purified with a silica gel column chromatography