反应详情

3.0 g of dihydroxyacetone dimer, 22.7 g of stearic acid, 16.8 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride salt, and 10.8 g of 4-dimethylaminopyridine were dissolved in 100 mL of dichloromethane, for overnight reaction under agitation at ambient temperature. Adding 0.5 L of methanol to the reaction solution, the generated powder was filtered and recovered. The powder recovered by filtration was washed with methanol. After the washed powder was dried, 6 g of the dried powder was dissolved in a mixture solution of 400 mL of tetrahydrofuran and 20 mL of aqueous 10% acetic acid solution, to which 1.1 g of sodium borohydride was added in small portions at 0° C. Subsequently, the resulting mixture was agitated at ambient temperature for 6 hours to promote the reaction. The resulting reaction solution was poured in saturated aqueous sodium hydrogen carbonate, for extraction in 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 3.5 g of the intended product.

1. customreaction under agitation at ambient temperature
2. filtrationthe generated powder was filtered
3. customrecovered
4. filtrationThe powder recovered by filtration
5. washwas washed with methanol
6. customAfter the washed powder was dried
7. dissolution6 g of the dried powder was dissolved in a mixture solution of 400 mL of tetrahydrofuran and 20 mL of aqueous 10% acetic acid solution, to which 1.1 g of sodium borohydride
8. additionwas added in small portions at 0° C
9. customthe reaction
10. customThe resulting reaction solution
11. customAfter the organic layer was dried
12. concentrationthe organic layer was concentrated under reduced pressure
13. customThe residue was purified by silica gel column chromatography