反应详情

Under reduced pressure of 60-70 mmHg and nitrogen gas stream, 250 g (0.71 mol) of methyl 5,9,13,17-tetramethyloctadec-4-enoate was slowly added dropwise at 78-83° C. to a solution of 157 g (1.15 mol) of pentaerythritol and 1.58 g (1.15 mmol) of potassium carbonate in dry N,N-dimethylformamide (700 mL). After the reaction mixture was stirred at the same temperature for 10 hours, formic acid was added at 75° C. to adjust the pH to 4. After the resulting solution was subjected to vacuum concentration, the residue was diluted with t-butylmethylether (1.5 L), and the resulting insoluble matter was separated by filtration. The filtrate was washed with 10% sodium bicarbonate aqueous solution twice, and decolorized with activated carbon (8 g). After filtration, the filtrate was concentrated, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate mixture) to obtain the title compound.

1. concentrationAfter the resulting solution was subjected to vacuum concentration
2. additionthe residue was diluted with t-butylmethylether (1.5 L)
3. customthe resulting insoluble matter was separated by filtration
4. washThe filtrate was washed with 10% sodium bicarbonate aqueous solution twice
5. filtrationAfter filtration
6. concentrationthe filtrate was concentrated
7. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate mixture)