Synthesis method of amikacin
A technology of amikacin and kanamycin, which is applied in the field of medicine, can solve the problems of increasing the amount of reaction solvent used, increasing the production cost, and easy volatilization of the solvent, so as to simplify the production equipment, facilitate the production operation, and reduce the use of solvents Effect
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[0057] Example 1
[0058] This embodiment provides a method for synthesizing amikacin, which includes the following steps:
[0059] 1) Catalytic silylation reaction: Put 600mL tetrahydrofuran into the silylation reaction flask, add 0.1 billion kanamycin (KMA), add 190mL hexamethyldisilazane (HMDS), add the catalyst triethylamine salt Salt 0.5g, start stirring, heat up to reflux, reflux for 130 minutes at 60~70℃, distill under reduced pressure, vacuum degree ≤-0.085Mpa, temperature 75-80℃ until no solvent flows out, silylation product;
[0060] 2) Acylation reaction: add 1000mL tetrahydrofuran to the silylation product, turn on the stirring, add 55g γ-N-phthalimido-α-hydroxybutyric acid (PHBA), add 48gN,N-bicyclohexyl Carbodiimide, control the temperature of the reactant at 25°C, and react for 120 minutes.
[0061] 3) Acidolysis reaction: After the acylation reaction is completed, turn on the stirring, add 350ml of 4.0mol / L hydrochloric acid, make the material pH 3.0, acidolyze at roo...
Example Embodiment
[0065] Example 2
[0066] This embodiment provides a method for synthesizing amikacin, which includes the following steps:
[0067] 1) Catalytic silylation reaction: put 600mL tetrahydrofuran into the silylation reaction flask, add 0.1 billion kanamycin (KMA), add 200mL hexamethyldisilazane (HMDS), add the catalyst diethylamine salt Salt 0.3g, start stirring, heat up to reflux, reflux for 110 minutes at 60-70°C, distill under reduced pressure, vacuum ≤-0.085Mpa, temperature 75-80°C until no solvent flows out, silylated product;
[0068] 2) Acylation reaction: add 1000mL tetrahydrofuran to the silylation product, turn on the stirring, add 60g γ-N-phthalimido-α-hydroxybutyric acid (PHBA), add 52gN,N-bicyclohexyl Carbodiimide, control the temperature of the reactant at 30°C, and react for 100 minutes.
[0069] 3) Acidolysis reaction: After the acylation reaction is completed, turn on the stirring, add 360ml of 4.0mol / L hydrochloric acid, make the material liquid pH 3.5, acidolyze at roo...
Example Embodiment
[0073] Example 3
[0074] This embodiment provides a method for synthesizing amikacin. The only difference from embodiment 1 is that in step 1), "catalyst triethylamine hydrochloride" is replaced with "triethylamine sulfate";
[0075] 1780 ml of amikacin synthetic liquid was obtained, and the amikacin content was 2.1% (g / ml) and the synthetic yield of kanamycin A was 31.3%.
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