Preparation method of salbutamol sulfate
A technology of salbutamol sulfate and salbutamol, which is applied in the preparation of organic compounds, cyanide reaction preparation, chemical instruments and methods, etc., can solve problems such as unsuitable for laboratory operation, difficult to realize industrialization, and difficult chiral separation, so as to avoid low temperature Or high temperature reaction, easy manipulation, and mild reaction conditions
Pending Publication Date: 2021-07-16
TIANJIN PHARMA GROUP CORP
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Problems solved by technology
[0010] The above three synthetic routes are long in the preparation process, cumbersome in operation, difficult in chiral resolution and low in yield, easy to introduce highly toxic dangerous goods, not suitable for laboratory operation, and difficult to realize industrialization
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Embodiment 1
[0071] The preparation of embodiment 1 intermediate 1
Embodiment 1-1
[0073]
Embodiment 1-1-1
[0075] Under the protection of nitrogen, add 150mL of toluene, 20g of salicylic acid and 26g of tert-butylaminoacetyl chloride into the reaction flask, stir and dissolve, then raise the temperature to 55°C, slowly add 32mL of thionyl chloride and 48mL of diisopropyl Ethylamine, after the dropwise addition, reacted at 55°C, and no salicylic acid was detected by TLC. After the reaction is complete, add water to separate the layers, wash the organic phase with saturated sodium chloride solution, dry over anhydrous sodium sulfate, concentrate under reduced pressure to about 20 mL, cool down to 0-5°C, and filter to obtain 35.9 g of intermediate 1-1. Yield 91.8%, HPLC content 99.5%.
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The invention provides a preparation method of salbutamol sulfate, and relates to the technical field of chemical synthesis. The preparation method of salbutamol sulfate comprises the following steps: (a) carrying out reaction on salicylic acid and a tert-butyl amino acetyl halogenating reagent under the action of a chlorinating agent to generate an intermediate 1; (b) reacting the intermediate 1 under the action of Lewis acid to generate an intermediate 2; (c) reacting the intermediate 2 under the action of an acid reagent to generate an intermediate 3; (d) reacting the intermediate 3 with a reducing agent under the action of a catalyst to generate salbutamol; and (e) reacting salbutamol with sulfuric acid to generate salbutamol sulfate. The raw materials are simple and easy to obtain, the reaction condition is mild, the reaction operation is simple, the reaction process is easier to control, and the safety coefficient is high; used raw materials, solvents and the like are environment-friendly; and the yield and purity of salbutamol sulfate are high, and a process route capable of industrially producing a product with higher quality is provided.
Description
technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of salbutamol sulfate. Background technique [0002] Salbutamol sulfate, chemical name 1-(4-hydroxy-3-hydroxymethylphenyl)-2-(tert-butylamino)ethanol sulfate. Salbutamol was developed by the British Glaxo Company in 1962, first listed in 1968, and registered in my country in 1988. Salbutamol sulfate is a β2-adrenergic receptor agonist. β2-adrenoceptors are mainly distributed in the surrounding small airways. As the diameter of the trachea becomes smaller, the distribution density becomes higher and higher. Bronchial smooth muscle relaxation, with a strong selective effect on β2-adrenergic receptors in bronchial smooth muscle. Salbutamol sulfate has become the drug of choice for the treatment of asthma and chronic obstructive pulmonary disease due to its good efficacy. [0003] The synthetic method of the salbutamol reported in the literature mai...
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IPC IPC(8): C07C213/08C07C215/60C07C213/00
CPCC07C213/00C07C213/08C07C227/22C07D223/14C07C215/60C07C229/38
Inventor 顾艳艳崔瞳晓
Owner TIANJIN PHARMA GROUP CORP
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