Improved process for preparing N6-benzoyl-D-adenosine
A technology of benzoyl and benzoyl chloride, applied in the field of nucleoside compounds
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Embodiment 1
[0050] Introduce nitrogen into the flask at a flow rate of 3L / h. Under stirring conditions, add 500g of pyridine, 100g of D-adenosine and 250g of hexamethyldisilazane in sequence, cool down to 0-5°C, and add 110g of trifluoroacetic acid-pyridine solution (The mass ratio of trifluoroacetic acid:pyridine is 1:10), and react for 1 hour to obtain a reaction system containing intermediate Ⅰ;
[0051] Slowly add 350g of benzoyl chloride to the reaction system of the prepared intermediate I, and control the temperature of the reaction system at 10-25°C during the addition process. After the addition, the temperature is kept at 20-25°C, and the reaction is stirred for 7 hours to obtain the intermediate II reaction system;
[0052] Add 500g of water to the reaction system of the prepared intermediate II, control the temperature of the system at 10-25°C, stir for 0.5 hours, add 400g of ammonia water with a concentration of 15-20% to the reaction system, the reaction temperature is ...
Embodiment 2
[0055] Feed nitrogen into the flask at a flow rate of 2L / h. Under stirring conditions, add 400g of pyridine, 100g of D-adenosine and 300g of hexamethyldisilazane in sequence, cool down to 0-5°C, and add 55g of trifluoroacetic acid-pyridine solution (The mass ratio of trifluoroacetic acid:pyridine is 1:10), and react for 1 hour to obtain a reaction system containing intermediate Ⅰ;
[0056] Slowly add 400 g of benzoyl chloride to the reaction system of the prepared intermediate I, and control the temperature of the reaction system to 10-25° C. during the addition process. After the addition, the temperature was kept at 20-25°C, and the reaction was stirred for 5 hours to obtain a reaction system containing intermediate II;
[0057] Add 200g of water to the reaction system of the prepared intermediate II, control the temperature of the system at 10-25°C, stir for 0.5 hours, add 300g of ammonia water with a concentration of 15-20% to the reaction system, the reaction tempe...
Embodiment 3
[0060] Introduce nitrogen into the flask at a flow rate of 3L / h. Under stirring conditions, add 500g of pyridine, 100g of D-adenosine and 250g of hexamethyldisilazane in sequence, cool down to 0-5°C, and add 110g of trifluoroacetic acid-pyridine solution (The mass ratio of trifluoroacetic acid:pyridine is 1:10), and react for 1 hour to obtain a reaction system containing intermediate Ⅰ;
[0061] Slowly add 350 g of benzoyl chloride to the reaction system of the prepared intermediate I, and control the temperature of the reaction system to 10-25° C. during the addition process. After the addition, the temperature was kept at 20-25°C, and the reaction was stirred for 7 hours to obtain a reaction system containing intermediate II;
[0062] Add 300g of water to the reaction system of the prepared intermediate II, control the temperature of the system at 10-25°C, stir for 0.5 hours, add 300g of ammonia water with a concentration of 15-20% to the reaction system, the reactio...
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