Preparation method for cytidine
A technology of cytidine nucleoside and cytosine, which is applied in the field of organic chemical synthesis, can solve the problems of high price and unsuitability for industrial production, and achieve the effect of low price, low cost and simple process steps
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[0046] Example 1
[0047] In a 250ml three-necked flask, add 10g of cytosine (0.09mol) and 150mg of ammonium sulfate, keep it dry, pass nitrogen protection into the three-necked flask, then add 30g (0.20mol) of tert-butyldimethylchlorosilane, and stir slowly. After the addition, the temperature is increased to 120°C and the reaction is kept for 8 hours. The product N-(tert-butyldimethylsilyl)-2-(tert-butyldimethylsiloxy)-4-pyrimidinamine is obtained. The product was dissolved with 100 ml of chloroform.
[0048] In a 250ml three-necked flask, add 35g (0.11mol) of tetraacetylribose and 10ml of chloroform and stir to dissolve, add 32g of titanium tetrachloride dropwise to it, and add dropwise N-(tert-butyl two The trichloromethane solution of methylsilyl)-2-(tert-butyldimethylsiloxy)-4-pyrimidinamine was dripped and stirred for 2h. After the reaction is complete, add 15ml of water, stir for 2h to quench, filter, and the filtrate is dried with anhydrous sodium sulfate and spin-dried...
Example Embodiment
[0052] Example 2
[0053] Add 10g (0.09mol) of cytosine (0.09mol) and 200mg of ammonium sulfate to a 250ml three-necked flask, keep it dry, pass helium gas into the three-necked flask, then add 27g (0.18mol) of tert-butyldimethylchlorosilane, and stir slowly . After the addition, the temperature is increased to 110°C and the reaction is kept for 10 hours, and the reaction is completed. The product N-(tert-butyldimethylsilyl)-2-(tert-butyldimethylsiloxy)-4-pyrimidinamine is obtained. The product was dissolved with 100 ml of chloroform.
[0054] In a 250ml three-necked flask, add 50g of tetraacetylribose (0.135mol) and 20ml of chloroform and stir to dissolve, add 60g of titanium tetrachloride dropwise to it, and add dropwise N-(tert-butyl two The trichloromethane solution of methylsilyl)-2-(tert-butyldimethylsiloxy)-4-pyrimidinamine was dripped and stirred for 5h. After the reaction is complete, add 15ml of water, stir for 2h to quench, filter, and the filtrate is dried with anhy...
Example Embodiment
[0058] Example 3
[0059] Add 10g of cytosine (0.09mol) and 100mg of ammonium sulfate to a 250ml three-necked flask, keep it dry, pour nitrogen into the three-necked flask, and then add 40.5g (0.27mol) of tert-butyldimethylchlorosilane and stir slowly . After the addition, the temperature is increased to 130°C and the reaction is kept for 6 hours. The product N-(tert-butyldimethylsilyl)-2-(tert-butyldimethylsilyloxy)-4-pyrimidinamine is obtained. The product was dissolved with 100 ml of chloroform.
[0060] In a 250ml three-necked flask, add 28.6g (0.09mol) of tetraacetylribose and 10ml of chloroform and stir to dissolve, add 28.6g of titanium tetrachloride dropwise to it, and add dropwise N-(tert-butyl) at an ambient temperature of 30℃. Dimethylsilyl)-2-(tert-butyldimethylsilyloxy)-4-pyrimidinamine in trichloromethane, dripped and stirred for 3.5h. After the reaction is complete, add 15ml of water, stir for 2h to quench, filter, and the filtrate is dried with anhydrous sodium ...
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