Method for preparing R-glyceraldehyde acetonide
A technology of glycerol aldehyde acetone and diacetone, which is applied in the direction of organic chemistry, can solve the problems of low product yield and purity, difficult recovery, long reaction steps, etc., to reduce the generation of by-products, short reaction route, and simple operation Effect
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Embodiment 1
[0019] Add 220g of dichloromethane, 23g of diacetone-D-mannitol, 0.23g of 18-crown-6-ether, and 0.4g of TEMPO into the clean reactor in sequence, stir and mix evenly, then slowly cool down to 10°C, and start adding mass Percentage is 10wt% sodium hypochlorite aqueous solution 72g, control the temperature of the reaction system below 15 ℃ during the dropwise addition, after the dropwise addition is completed, continue the reaction to keep the temperature at 30 ℃ ~ 32 ℃ for oxidation reaction for 1h, after the reaction , stand still, separate layers, remove the water layer, wash the collected organic layer once with 50g water, remove the water layer layer by layer, add 20g of anhydrous sodium sulfate to the collected organic layer, stir and carry out drying treatment for 30min, suction filter, collect the filtrate, and The filtrate was concentrated under reduced pressure to remove the solvent, and the obtained wet product was dried to obtain 22.1 g of dry product R-glyceraldehyde...
Embodiment 2
[0021] Add 300g of dichloromethane, 23g of diacetone-D-mannitol, 0.4g of 18-crown-6-ether, and 0.6g of TEMPO into a clean reactor in sequence, stir and mix well, then slowly cool down to 15°C, and start to add mass The percentage is 80g of sodium hypochlorite aqueous solution with a percentage of 10wt%, and the temperature of the reaction system is controlled below 15°C during the dropwise addition. Finally, let stand, separate layers, remove the water layer, wash the collected organic layer once with 50g water, remove the water layer layer by layer, add 20g of anhydrous sodium sulfate to the collected organic layer, stir and carry out drying treatment for 30min, suction filtration, collect the filtrate, The filtrate was concentrated under reduced pressure to remove the solvent, and the obtained wet product was dried to obtain 22 g of dry product R-glycerol aldehyde acetone with a yield of 96.5% and a gas phase content of 99.4%.
Embodiment 3
[0023] Add 200g of ethyl acetate, 23g of diacetone-D-mannitol, 0.6g of 15-crown-5-ether, and 0.5g of TEMPO into the clean reactor in turn, stir and mix well, then slowly cool down to 5°C, and start to drop the mass The percentage is 10wt% calcium hypochlorite aqueous solution 140g, control the temperature of the reaction system below 5°C during the dropwise addition, after the dropwise addition is completed, continue the reaction and keep the temperature at 5°C-10°C for 1.5h of oxidation reaction , after the reaction was finished, let stand, separate layers, remove the water layer, wash the collected organic layer once with 50g water, remove the water layer layer by layer, add 20g of anhydrous sodium sulfate to the collected organic layer, stir and carry out drying treatment for 30min, suction filtration, The filtrate was collected, and the filtrate was concentrated under reduced pressure to remove the solvent. After drying the obtained wet product, 22.3 g of dry product R-glyc...
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