Method for preparing cigarette fragrance releaser with honey sweet note
A technology of releasing agent and aroma, which is applied in the field of preparation of flavor releasing agent for cigarettes, can solve the problems of low yield of target product and many losses of intermediate products, and achieves high yield, reduced product loss and good thermal stability. Effect
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Embodiment 1
[0028] Preparation of α-bromotetraacetylglucose: Add 3.6g of glucose to 80g of acetic anhydride, acetylate under the catalysis of 0.05mL perchloric acid to obtain acetylated glucose solution, slowly add 8g of acetylated glucose to the obtained acetylated glucose solution Saturated hydrogen bromide solution (add within 30 minutes, the mass ratio of glucose, acetic anhydride and hydrogen bromide solution is 1:22.2:2.2), hydrogen bromide reacts with acetylated glucose to generate α-bromotetraacetyl The reaction mixture was diluted with 40 mL of ethyl acetate, washed successively with 50 mL of ice-cold brine and 50 mL of saturated potassium bicarbonate solution, the organic phase was separated, dried, and concentrated to obtain the crude product of α-bromotetraacetylglucose, which was reconstituted with ether. The product α-bromotetraacetylglucose was obtained by crystallization with a yield of 96%.
Embodiment 2
[0030] Preparation of α-bromotetraacetylglucose: Add 3.6g of glucose to 60g of acetic anhydride, acetylate under the catalysis of 0.05mL perchloric acid to obtain acetylated glucose solution, slowly add 10.5 g saturated hydrogen bromide solution (add within 30 minutes, the mass ratio of glucose, acetic anhydride and saturated hydrogen bromide solution is 1:16.7:2.9), hydrogen bromide reacts with acetylated glucose for 30 minutes at 15°C to form α-Bromotetraacetylglucose, after the reaction, dilute the reaction mixture with 40mL ethyl acetate, wash with 50mL ice brine, 50mL saturated potassium bicarbonate solution successively, separate the organic phase, and then wash the organic phase over anhydrous sodium sulfate Dry and concentrate to obtain the crude product of α-bromotetraacetylglucose, which is recrystallized with ether to obtain the product α-bromotetraacetylglucose with a yield of 90%.
[0031] Comparative Example of Examples 1 and 2
[0032] According to the classic ...
Embodiment 3
[0034]Preparation of reaction intermediate benzyl-tetraacetyl-β-D-glucopyranoside: 3.6g glucose was added to 80g acetic anhydride, acetylated under the catalysis of 0.05mL perchloric acid to obtain acetylated glucose solution, Slowly add 5.8g of saturated hydrogen bromide solution to the acetylated glucose solution (completely add within 30 minutes), and react hydrogen bromide with acetylated glucose for 10 minutes at 25°C to generate α-bromotetraacetylglucose, and the reaction ends Finally, dilute the reaction mixture with 40mL ethyl acetate, wash with 50mL ice brine and 50mL saturated potassium bicarbonate solution successively, separate the organic phase, then dry the organic phase over anhydrous sodium sulfate and concentrate to obtain α-bromotetraacetyl base glucose crude product; it was mixed with 2.2g benzyl alcohol, 2.3g silver oxide, 4g 4A molecular sieves, 40mL ethyl acetate, and reacted in the dark at room temperature for 48 hours; the reacted mixture was filtered, a...
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