A kind of synthetic method of ester compound
The technology of an ester compound and a synthesis method, which is applied in the synthesis field of the ester compound, can solve the problems of waste of resources, environment, pollution, etc., and achieves the effects of short reaction time, broad application prospects, and cheap and easily available raw materials
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Embodiment 1
[0011]
[0012] Add p-methoxybenzaldehyde (1a, 0.5mmol, 68mg), bromo-n-butane (2a, 1mmol, 137mg), water (2mL), tert-butyl hydroperoxide (1mmol, 138μL) into a 25mL pressure-resistant tube , 70wt% aqueous solution) and tetrabutylammonium iodide (0.5mmol, 184mg), then the pressure tube was sealed and placed in an oil bath, and stirred at 80°C for 2 hours. After the reaction was completed, 10 mL of water was added, extracted with ethyl acetate (10 mL×3), the combined organic phases were washed with Na 2 S 2 o 3 Washed with aqueous solution, then dried over anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, the product was separated on a silica gel column (petroleum ether / ethyl acetate=30 / 1) to obtain the product 3a (75 mg, 72%) as a colorless oil. The characterization data of this compound are as follows: 1 H NMR (400MHz, CDCl 3 )δ: 0.89(t, J=7.2Hz, 3H), 1.34-1.43(m, 2H), 1.62-1.69(m, 2H), 3.77(s, 3H), 4.21(t, J=6.8Hz, 2H ),6.81-6.85(m,2...
Embodiment 2
[0014] Add p-methoxybenzaldehyde (1a, 0.5mmol, 68mg), bromo-n-butane (2a, 1mmol, 137mg), acetonitrile (2mL), tert-butyl hydroperoxide (0.5mmol, 69μL, 70wt% aqueous solution) and tetrabutylammonium iodide (0.1mmol, 37mg), then the pressure tube was sealed and placed in an oil bath, and stirred at 80°C for 2 hours. After the reaction was completed, 10 mL of water was added, extracted with ethyl acetate (10 mL×3), the combined organic phases were washed with Na 2 S 2 o 3 Washed with aqueous solution, then dried over anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, the product was separated on a silica gel column (petroleum ether / ethyl acetate=30 / 1) to obtain the product 3a (23 mg, 22%) as a colorless oil.
Embodiment 3
[0016] Add p-methoxybenzaldehyde (1a, 0.5mmol, 68mg), bromo-n-butane (2a, 1mmol, 137mg), acetonitrile (2mL), tert-butyl hydroperoxide (1mmol, 138μL) into a 25mL pressure tube , 70wt% aqueous solution) and tetrabutylammonium iodide (0.1mmol, 37mg), then the pressure tube was sealed and placed in an oil bath, and stirred at 80°C for 2 hours. After the reaction was completed, 10 mL of water was added, extracted with ethyl acetate (10 mL×3), the combined organic phases were washed with Na 2 S 2 o 3 Washed with aqueous solution, then dried over anhydrous sodium sulfate. After the solvent was distilled off under reduced pressure, the product was separated on a silica gel column (petroleum ether / ethyl acetate=30 / 1) to obtain the product 3a (33 mg, 32%) as a colorless oil.
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