反应详情

After dissolving 7.0 g of sodium hydroxide in 50 ml of water and 50 ml of ethanol at 4° C., 10.7 g of nitromethane and 10.0 g of 2-methylpentanal were added thereto. The temperature of the solution was allowed to rise to room temperature, and the solution was stirred for two hours. After concentrating the ethanol under reduced pressure, the solution was neutralized with 1 mol/l of hydrochloric acid so that the pH of the solution was approximately 7. Ethyl acetate was added to the solution, and the organic layer was washed with saturated saline. The organic layer was dried with magnesium sulfate and concentrated, and then purified by silica gel chromatography (hexane/ethyl acetate=8/1), thereby obtaining 13.3 g of 3-methyl-1-nitro-2-hexanol (yield: 94.2%).

1. customto rise to room temperature
2. concentrationAfter concentrating the ethanol under reduced pressure
3. additionEthyl acetate was added to the solution
4. washthe organic layer was washed with saturated saline
5. dry with materialThe organic layer was dried with magnesium sulfate
6. concentrationconcentrated
7. custompurified by silica gel chromatography (hexane/ethyl acetate=8/1)