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ChemicalBook CAS DataBase List Etamsylate
2624-44-4

Etamsylate synthesis

2synthesis methods
Nowadays, the production methods of etamsylate in the market are benzoquinone method, in which benzoquinone method is to pass sulfur dioxide in the solution of diethylamine, ethanol and water, and then make diethylamine sulfite salt, then add p-benzoquino
-

Yield:2624-44-4 85%

Reaction Conditions:

in cyclohexane at 65 - 70;Solvent;Temperature;

Steps:

1; 2; 3 Example 3
To a 10 L enamel reactor was added 1.65 kg of hydroquinone, 4.5 L of cyclohexane, and 0.2 L of propionic acid.The mixture was heated to reflux with stirring, and refluxed for 2 h.After the water is separated, the temperature is lowered to micro reflux, and the internal temperature of the reactor is 85 ° C.Add 2.28kg concentrated sulfuric acid, control the internal temperature of the reaction kettle does not exceed 90 ° C;After the addition, the temperature was maintained at 90 ° C for 60 min.Stop heating, pass the cooling water to cool down to the lower paste temperature 65 ° C,A mixture of 1.25 kg of diethylamine and 0.9 L of water was added dropwise.Control the internal temperature of the reaction vessel to be added dropwise at 65 ° C, and the maximum height of the reaction vessel should not exceed 70 ° C;After the completion of the dropwise addition, the temperature is raised to 70 ° C to stir and dissolve the lower aqueous phase, and the hot liquid is separated;The aqueous phase was collected, transferred to a 10 L reaction kettle, slowly cooled to about 10 ° C, stirred and decanted for 1 h, then cooled to 5 ° C, stirred and decanted for 8 h, then centrifuged for centrifugation, centrifuged to dryness and then filtered cake with 1.5 L. Washing with propanol, 1.5L of isopropanol each time, a total of three times of beating,The white crystalline particulate solid phenolsulfonamide was obtained in an amount of 3.35 kg, the yield was 85%, and the purity was 99.89%. The obtained phenolsulfonamide was analyzed by high performance liquid chromatography, and the results obtained are shown in Fig. 4.

References:

Chengdu Pinghe Good Health Pharmaceutical Technology Co., Ltd.;Jin Lei;Lu Jie;Ni Ying;Zhang Ling;Zhang Weiqun CN109467522, 2019, A Location in patent:Paragraph 0025; 0029-0036

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