Preparation method for 5-hydroxymethylfurfural
A technology of hydroxymethyl furfural and dimethyl sulfoxide, applied in the field of preparation of 5-hydroxymethyl furfural, can solve the problems of unsuitability for mass production, high catalyst toxicity, adhesion of by-products, etc., and avoid highly toxic chemical raw materials The use of the substrate, the wide range of substrates, and the effect of mild reaction conditions
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Embodiment 1
[0016] 1 g (2.92 mmol) sucrose and 406 mg (0.56 mmol) FeCl 3 ·6H 2 O / C (1:3) was dissolved in 10 mL of acetonitrile, and stirred and heated at 60°C, reacted for 6 hours, and the reaction was terminated after the complete conversion of sucrose was monitored by TLC (chloroform / methanol / water=3:3:1). Then the catalyst in the reaction system was filtered out, washed with ethyl acetate (EtOAc), recovered and recycled. The combined filtrate and washing liquid were washed with saturated brine, the organic phase was separated, and the aqueous phase was extracted several times with ethyl acetate. After the organic phase was combined, the organic phase was washed again with saturated brine and the organic phase was separated. After drying with sodium sulfate, rotary evaporation under reduced pressure and separation and purification by column chromatography gave 478 mg of 5-hydroxymethylfurfural with a yield of 65%.
Embodiment 2
[0018] 1 g (5.6 mmol) of glucose and 406 mg (0.56 mmol) of FeCl 3 ·6H 2 O / C (1:5) was dissolved in 10 mL polyethylene glycol 400, stirred and heated at 100°C, and reacted for 6 hours. The reaction was completed after the complete conversion of glucose was monitored by TLC, and then the catalyst in the reaction system was filtered out. Wash with ethyl acetate (EtOAc), recover and recycle. The combined filtrate and washing liquid were washed with saturated brine, the organic phase was separated, and the aqueous phase was extracted several times with ethyl acetate. After the organic phase was combined, the organic phase was washed again with saturated brine and the organic phase was separated. After drying over magnesium sulfate, concentrate under reduced pressure and separate and purify by column chromatography to obtain 353 mg of 5-hydroxymethylfurfural with a yield of 50%.
Embodiment 3
[0020] Mix 1 g (5.6 mmol) fructose and 406 mg (0.56 mmol) FeCl 3 ·6H 2 O / C (1:1) was dissolved in 10 mL dimethyl sulfoxide (DMSO), heated at 80°C for 3 hours, and the reaction was completed after the conversion of fructose was monitored by TLC, then the catalyst in the reaction system was filtered out, and used Ethyl acetate (EtOAc) washing, recovery and recycling. The combined filtrate and washing liquid were washed with saturated brine, the organic phase was separated, and the aqueous phase was extracted several times with ethyl acetate. After the organic phase was combined, the organic phase was washed again with saturated brine and the organic phase was separated. After drying over sodium sulfate, vacuum rotary evaporation and column chromatography separation and purification gave 593 mg of 5-hydroxymethylfurfural, with a yield of 84%.
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