Method for preparing darunavir
A technology of darunavir and ferric nitrite, applied in organic chemistry and other directions, can solve the problems of high price of darunavir, high requirements for preparation environment, and patients cannot afford the price.
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Embodiment 1
[0021] Embodiment one: a kind of preparation method of darunavir comprises the following steps:
[0022] 1) Take 20 parts of cobalt, 10 parts of triethylamine, 10 parts of ferrous oxide, 10 parts of zinc oxide, 3 parts of 1.2 equivalents of hydrogen methane, 20 parts of zinc, 50 parts of ferric nitrite solution, 30 parts of metal alkali, and 40 parts of aluminum, 10 parts of silicon dioxide, 3 parts of p-acetamidobenzoyl sulfonyl chloride, 3 parts of precipitant, 50 parts of ethanol solution and 20 parts of nickel for later use;
[0023] 2) Take 50 parts of ferric nitrite solution and place it in a reaction vessel, put 20 parts of nickel, 20 parts of cobalt and 20 parts of zinc into 50 parts of ferric nitrite solution, adjust the reaction temperature to be 50 degrees Celsius, and use a stirring device to stir for 1-2 hour, set the stirring frequency as one hundred and twenty revolutions per minute, and make the mixed solution 1;
[0024] 3) Add 40 parts of alumina and 10 part...
Embodiment 2
[0031] Embodiment 2: a preparation method of darunavir, comprising the following steps:
[0032] 1) Take 25 parts of cobalt, 15 parts of triethylamine, 15 parts of ferrous oxide, 15 parts of zinc oxide, 4 parts of 1.2 equivalents of hydrogen methane, 25 parts of zinc, 65 parts of ferric nitrite solution, 35 parts of metal alkali, and 45 parts of aluminum, 15 parts of silicon dioxide, 4 parts of p-acetamidobenzoyl sulfonyl chloride, 4 parts of precipitant, 65 parts of ethanol solution and 25 parts of nickel for subsequent use;
[0033] 2) Get 65 parts of ferric nitrite solution and place it in a reaction vessel, put 25 parts of nickel, 25 parts of cobalt and 25 parts of zinc into ferric nitrite solution 65, adjust the reaction temperature to be 50 degrees Celsius, and use a stirring device to stir for 1-2 hour, set the stirring frequency as one hundred and twenty revolutions per minute, and make the mixed solution 1;
[0034] 3) Add 45 parts of alumina and 15 parts of silicon ...
Embodiment 3
[0040] Embodiment three: a preparation method of darunavir, comprising the following steps:
[0041] 1) Take 30 parts of cobalt, 20 parts of triethylamine, 20 parts of ferrous oxide, 20 parts of zinc oxide, 5 parts of 1.2 equivalents of hydrogen methane, 30 parts of zinc, 80 parts of ferric nitrite solution, 40 parts of metal alkali, and 50 parts of aluminum, 20 parts of silicon dioxide, 5 parts of p-acetamidobenzoyl sulfonyl chloride, 5 parts of precipitant, 80 parts of ethanol solution and 30 parts of nickel for standby;
[0042] 2) Take 80 parts of ferric nitrite solution and place it in a reaction vessel, put 30 parts of nickel, 30 parts of cobalt and 30 parts of zinc into 80 parts of ferric nitrite solution, adjust the reaction temperature to be 50 degrees Celsius, and use a stirring device to stir for 1-2 hour, set the stirring frequency as one hundred and twenty revolutions per minute, and make the mixed solution 1;
[0043] 3) Add 50 parts of alumina and 20 parts of s...
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