Vidarabine synthesis method
A vidarabine adenosine and synthetic method technology, which is applied in the direction of chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve the problems of harsh desulfurization conditions and increased production costs, and achieve improved safety, improved activity, The effect of reducing the content of heavy metals
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Embodiment 1
[0021] First, add 10g (0.019mol) 8-hydroxy-N,3',5'-O-triethyl-2'-O-p-toluenesulfonyladenosine (1) and 13g mass concentration to a 250mL three-necked flask It is 80% hydrazine hydrate, heat up to 78°C and keep it warm for 50 hours. The initial raw material in the reaction solution is detected by high performance liquid phase, namely 8-hydroxy-N,3',5'-O-triethyl-2'-O-p-toluenesulfonate When the acyladenosine content was 0.96%, the reaction was terminated.
[0022] Then, after removing four-fifths of hydrazine hydrate by distillation under reduced pressure, add 10 g of hot water at 55°C to the reaction flask, continue the reduced-pressure distillation, and take out the hydrazine hydrate remaining in the reaction flask, and the remaining solid is 8- The crude product of hydrazino vidarabine (2).
[0023] Then, in the same reaction flask, continue to add 50 g of water and 0.3 g of potassium permanganate to the crude product of 8-hydrazino vidarabine, stir and react for 8 hours at ...
Embodiment 2
[0026] First, add 100g (0.192mol) 8-hydroxy-N,3',5'-O-triethyl-2'-O-p-toluenesulfonyladenosine (1) and 120g mass concentration to a 2L three-necked flask It is 80% hydrazine hydrate, heat up to 80°C and keep it warm for 48 hours, and detect 8-hydroxy-N,3',5'-O-triethyl-2'-O-p-toluenesulfonyladenosine in the reaction solution by high performance liquid phase When the content of is 0.96%, finish reaction.
[0027] Then, after removing four-fifths of hydrazine hydrate by distillation under reduced pressure, add 100 g of hot water at 60°C to the reaction flask, continue the reduced-pressure distillation, and take out the hydrazine hydrate remaining in the reaction flask, and the remaining solid is 8- The crude product of hydrazino vidarabine (2).
[0028] Then, in the same reaction flask, continue to add 600 g of water and 6 g of potassium permanganate to the obtained 8-hydrazino vidarabine crude product, stir and react at room temperature for 7 hours, and detect the 8-hydrazino ...
Embodiment 3
[0031] First, add 1kg (1.92mol) 8-hydroxy-N,3',5'-O-triethyl-2'-O-p-toluenesulfonyladenosine (1) and 1.3kg mass concentration to the 20L reactor It is 80% hydrazine hydrate, heat up to 85°C and keep it warm for 45 hours, and detect 8-hydroxy-N,3',5'-O-triethyl-2'-O-p-toluenesulfonyladenosine in the reaction solution by high performance liquid phase When the content was 0.95%, the reaction was terminated.
[0032] Then, after removing four-fifths of the hydrazine hydrate by distillation under reduced pressure, add 1 kg of hot water at 65°C to the reaction kettle, continue the distillation under reduced pressure, and take out the hydrazine hydrate remaining in the kettle, and the remaining solid is 8-hydrazine Vidarabine (2) crude product.
[0033] Then, in the same reaction kettle, continue to add 7kg water and 90g potassium permanganate to the crude product of 8-hydrazino vidarabine, stir and react at room temperature for 6h, and detect the 8-hydrazino vidarabine in the react...
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