反应详情

温度

75 °C

1-Acetoxy-4-chloro-3-methyl-2-butene (7.8 g) was added to a suspension of hexamine (6.7 g) and acetonitrile (47 ml), and the mixture was stirred at room temperature for 16 hours. The precipitated crystals were separated by filtration to give crystals (12.5 g) of a quaternary ammonium salt. This salt (7.9 g) was dissolved in water (50 ml), and toluene (100 ml) was added. With stirring at 75° C., acetic acid (1.5 g per addition) was added 30 minutes, 1 hour and 2 hours after the beginning of the reaction. The reaction was stopped 6 hours after the beginning of the reaction. The toluene layer was separated and concentrated, and the resulting residue was purified by column chromatography on silica gel to give 4-acetoxy-2-methyl-2-buten-1-al (2.6 g, 74%).

1. customafter the beginning of the reaction
2. customafter the beginning of the reaction
3. customThe toluene layer was separated
4. concentrationconcentrated
5. customthe resulting residue was purified by column chromatography on silica gel