Utilization method of 2-hydroxy-1,3,5-tri-o-benzoyl-α-d-ribofuranose crystallization mother liquor
A benzoyl and ribofuranose technology, applied in chemical instruments and methods, sugar derivatives, sugar derivatives and other directions, can solve the problems of high solubility and only 40-50% yield, and achieves simple operation and reduced production costs. , the effect of low cost
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Embodiment 1
[0023] Take 2-hydroxy-1,3,5-tri-O-benzoyl-α-D-ribofuranose and its isomer 1-hydroxy-2,3,5-tri-O-benzoyl-D - 200ml of the mother liquor of 20g of ribofuranose, concentrated to dryness under reduced pressure below 35°C, then added 40ml of acetone and 17ml of acetic anhydride to dissolve the concentrate, lowered the temperature to below 0°C, slowly added 2ml of concentrated sulfuric acid, and stirred at 0-5°C Heat preservation reaction for 6 hours.
[0024] After the heat preservation reaction was completed, 80ml of ice water was slowly added, and the temperature was controlled below 5°C, and a white solid was formed. Stir at 15-25°C for 2 hours and then filter with suction to obtain 22.6g of crude product with a HPLC purity of 93.1%; heat and dissolve the obtained solid with 100ml of ethanol, after the dissolution is complete, add 5g of silica gel and 1g of activated carbon, and keep stirring at 70-80°C for 30 Minutes; filter while hot, wash the filter cake with a small amount ...
Embodiment 2
[0027] Take 2-hydroxy-1,3,5-tri-O-benzoyl-α-D-ribofuranose and its isomer 1-hydroxy-2,3,5-tri-O-benzoyl-D - 200ml of the mother liquor of 20g of ribofuranose, concentrated to dryness under reduced pressure below 35°C, then added 40ml of acetonitrile and 17ml of acetic anhydride to dissolve the concentrate, lowered the temperature to below 0°C, slowly added 2ml of concentrated sulfuric acid, and stirred at 0-5°C Heat preservation reaction for 6 hours.
[0028] After the heat preservation reaction was completed, 80ml of ice water was slowly added, and the temperature was controlled below 5°C, and a white solid was formed. Stir at 15-25°C for 2 hours and then filter with suction to obtain 21.4g of crude product with HPLC purity of 93.7%; heat and dissolve the obtained solid with 100ml of ethanol. Minutes; filter while hot, wash the filter cake with a small amount of hot ethanol, wash the filtrate to cool to room temperature, then cool and stir in an ice-water bath for 2 hours. ...
Embodiment 3
[0031] Take 2-hydroxy-1,3,5-tri-O-benzoyl-α-D-ribofuranose and its isomer 1-hydroxy-2,3,5-tri-O-benzoyl-D - 200ml of mother liquor of 20g of ribofuranose, concentrated to dryness under reduced pressure below 35°C, then added 40ml of 1,4-dioxane and 17ml of acetic anhydride to dissolve the concentrate, lowered the temperature to below 0°C, slowly added 2ml of concentrated sulfuric acid, and Stir and keep warm at 0-5°C for 6 hours.
[0032]After the heat preservation reaction was completed, 80ml of ice water was slowly added, and the temperature was controlled below 5°C, and a white solid was formed. Stir at 15-25°C for 2 hours and then filter with suction to obtain 21.2g of crude product with HPLC purity of 91.7%; heat and dissolve the obtained solid with 100ml of ethanol, after the dissolution is complete, add 5g of silica gel and 1g of activated carbon, and keep stirring for 30 Minutes; filter while hot, wash the filter cake with a small amount of hot ethanol, wash the filtr...
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