反应详情

温度

-25 °C

To a solution of methyl 9-oxononanate (5.26 g) in THF (60 ml) was dropwise added 0.95M vinyl magnesium bromide (31.1 ml) at −30° C. and then stirred for 30 minutes at −25° C. The reaction mixture was poured into saturated ammonium chloride aqueous solution and then extracted with diethyl ether. The organic layer was washed with saturated brine, dried over magnesium sulfate anhydride, and then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1) to give methyl 9-hydroxy-10-undecenate (3.41 g, 56.3%).

1. customat −30° C.
2. extractionextracted with diethyl ether
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over magnesium sulfate anhydride
5. customevaporated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1)