A flavoring and moisturizing agent 1-l-tryptophan-1-deoxy-d-fructose for tobacco and its preparation method
A technology of moisturizing agent and tryptophan for cigarettes, applied in the preparation of sugar derivatives, chemical instruments and methods, tobacco and other directions, can solve the problems of unsatisfactory improvement effect of smoking comfort, and achieve the effect of reasonable synthesis route
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Embodiment 1
[0025] The preparation method of 1-L-tryptophan-1-deoxy-D-fructose, it comprises the steps:
[0026] Weigh 0.06mol of D-mannose into a 500mL three-neck flask, add 168mL of anhydrous methanol, magnetically stir and reflux for 20 minutes, then add 0.048mol of tryptophan and 0.0012mol of citric acid in sequence, and then reflux for another 4 hours to end the reaction. After the reaction solution was cooled to room temperature, the unreacted D-mannose and amino acids were filtered off, and then concentrated under reduced pressure, separated by strong acid ion exchange resin column chromatography and recrystallized to obtain 8.765 g of the white target product with a yield of 39.89%.
[0027] When separating, first add the synthetic sample aqueous solution to the resin column, and then use distilled water to wash off impurities such as unreacted D-mannose and uncharged substances, and then use 1mol / L HCl aqueous solution to wash, and use a specific method to wash at any time. Monit...
Embodiment 2
[0029] The preparation method of 1-L-tryptophan-1-deoxy-D-fructose, it comprises the steps:
[0030] Weigh 0.06mol of D-mannose into a 500mL three-necked flask, add 200mL of anhydrous methanol, magnetically stir and reflux for 30min, then add 0.06mol of tryptophan and 0.0024mol of citric acid in sequence, and then reflux for 5.5h to end the reaction. After the reaction liquid was cooled to room temperature, the unreacted D-mannose and amino acid were filtered off, then concentrated under reduced pressure, separated by strong acid ion exchange resin column chromatography and recrystallized to obtain 14.834 g of the white target product with a yield of 67.52%.
[0031] When separating, first add the synthetic sample aqueous solution to the resin column, and then use distilled water to wash off impurities such as unreacted D-mannose and uncharged substances, and then use 1mol / L HCl aqueous solution to wash, and use a specific method to wash at any time. Monitor the eluent, when t...
Embodiment 3
[0033] The preparation method of 1-L-tryptophan-1-deoxy-D-fructose, it comprises the steps:
[0034] Weigh 0.06mol of D-mannose into a 500mL three-neck flask, add 240mL of anhydrous methanol, magnetically stir and reflux for 40min, then add 0.072mol of tryptophan and 0.003mol of citric acid in sequence, and then reflux for another 7h to end the reaction. After the reaction solution was cooled to room temperature, the unreacted D-mannose and amino acid were filtered off, then concentrated under reduced pressure, separated by strong acid ion exchange resin column chromatography and recrystallized to obtain 10.032 g of the white target product with a yield of 45.66%.
[0035] When separating, first add the synthetic sample aqueous solution to the resin column, and then use distilled water to wash off impurities such as unreacted D-mannose and uncharged substances, and then use 1mol / L HCl aqueous solution to wash, and use a specific method to wash at any time. Monitor the eluent, ...
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