反应详情

3.8 g of dihydroxyacetone dimer, 25 g of oleic acid, g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride salt, and 12.9 g of 4-dimethylaminopyridine were dissolved in 150 mL of dichloromethane, for reaction under agitation at ambient temperature for 4 hours. The organic layer was washed by adding aqueous 0.5 M potassium dihydrogen phosphate solution to the reaction solution. After the organic layer was dried and concentrated under reduced pressure, 1 L of methanol was added to the resulting residue; the generated powder was filtered and recovered, and then dried. The dried powder was dissolved in a mixture solution of 170 mL of tetrahydrofuran and 17 mL of aqueous 10% acetic acid solution, to which 1.7 g of sodium borohydride was added in small portions at 0° C. Subsequently, the resulting mixture was agitated at ambient temperature for 2 hours to promote the reaction. The resulting reaction solution was poured in saturated aqueous sodium hydrogen carbonate, for extraction with ethyl acetate. After the organic layer was dried, the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography, to obtain 14.5 g of the intended product.

1. washThe organic layer was washed
2. additionby adding aqueous 0.5 M potassium dihydrogen phosphate solution to the reaction solution
3. customAfter the organic layer was dried
4. concentrationconcentrated under reduced pressure, 1 L of methanol
5. additionwas added to the resulting residue
6. filtrationthe generated powder was filtered
7. customrecovered
8. customdried
9. dissolutionThe dried powder was dissolved in a mixture solution of 170 mL of tetrahydrofuran and 17 mL of aqueous 10% acetic acid solution, to which 1.7 g of sodium borohydride
10. additionwas added in small portions at 0° C
11. customthe reaction
12. customThe resulting reaction solution
13. customAfter the organic layer was dried
14. concentrationthe organic layer was concentrated under reduced pressure
15. customThe residue was purified by silica gel column chromatography