反应详情

After dissolving 15.0 g of 3-methyl-1-nitro-2-hexanol in 100 ml of dichloromethane, 11.7 g of mesyl chloride and 18.8 g of triethylamine were gradually dropped thereto at 4° C., respectively. The temperature of the solution was allowed to rise to room temperature, and the solution was stirred for an hour. Water was added to stop the reaction, and the solution was extracted with dichloromethane. The organic layer was dried with magnesium sulfate and concentrated, and then purified by silica gel chromatography (hexane/ethyl acetate=10/1), thereby obtaining 9.0 g of 3-methyl-1-nitrohex-1-ene (yield: 81.4%).

1. additionwere gradually dropped
2. customat 4° C.
3. customto rise to room temperature
4. customthe reaction
5. extractionthe solution was extracted with dichloromethane
6. dry with materialThe organic layer was dried with magnesium sulfate
7. concentrationconcentrated
8. custompurified by silica gel chromatography (hexane/ethyl acetate=10/1)