Preparation method of doxycycline hydrochloride intermediate hydride

A technology of doxycycline hydrochloride and preparation process, which is applied in the preparation of organic compounds, the preparation of sulfonates, the preparation of carboxylic acid amides, etc., can solve the problem that the recovery difficulty of sodium tosylate and sodium sulfosalicylate is increased, and the production Cost increase and other problems, to achieve the effect of reducing the cost of three waste treatment, reducing the difficulty of recycling, and improving the recovery rate and product purity

Active Publication Date: 2017-06-16
昆山华苏生物科技有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0003] It can be seen that in the traditional method for preparing doxycycline hydrochloride intermediate hydride, oxytetracycline chloride needs to be salified with a large amount of p-toluenesulfonic acid, crystallized, and

Method used

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  • Preparation method of doxycycline hydrochloride intermediate hydride
  • Preparation method of doxycycline hydrochloride intermediate hydride
  • Preparation method of doxycycline hydrochloride intermediate hydride

Examples

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Embodiment 1

[0027] Oxytetracycline generates chlorinated products after chlorination reaction, and the chlorinated products are air-dried to remove methanol. Inhale 100 kg of dried chlorinated substances into the dehydration reaction pot, prepare 150 kg of HF in the dehydration reaction pot according to the weight ratio of HF:chlorinated compounds at 1.5:1, and pre-cool it to below -20°C with a frozen brine jacket. Stir while inhaling the chlorinated compound, control the reaction temperature after absorbing the chlorinated compound to be 5-10°C, continue to stir and react for 8 hours, stop stirring, and let stand for 6 hours. The dehydrated feed liquid after the reaction is concentrated by a falling film evaporator to remove HF. The concentrated liquid can be received with 200L of methanol in the receiving tank, and the 200L of methanol is pre-cooled to below 0°C with a frozen brine jacket, and then received while stirring, and the temperature of the methanol solution receiving the conce...

Embodiment 2

[0032] Oxytetracycline generates chlorinated products after chlorination reaction, and the chlorinated products are air-dried to remove methanol. Inhale 100 kg of dried chlorinated substances into the dehydration reaction pot, prepare 200 kg of HF in the dehydration reaction pot according to the weight ratio of HF:chlorinated compounds at 2:1, and pre-cool it to below -20°C with a frozen brine jacket. Stir while inhaling the chlorinated compound, control the reaction temperature after absorbing the chlorinated compound to be 0-5°C, continue to stir and react for 10 hours, stop stirring, and let stand for 8 hours. The dehydrated feed liquid after the reaction is concentrated by a falling film evaporator to remove HF. The concentrated liquid is received with 300L methanol in the receiving tank, and the 300L methanol is pre-cooled to below 0°C with a chilled brine jacket, and then received while stirring, and the temperature of the methanol solution receiving the concentrated liq...

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Abstract

The invention discloses a preparation method of a doxycycline hydrochloride intermediate hydride. The preparation method comprises adding dried oxytetracycline chloride into a dehydration pot containing HF, carrying out reaction dehydration, carrying out standing, evaporating and concentrating to remove HF, collecting the concentrated solution through methanol, neutralizing the methanol solution containing the concentrated solution through calcium hydroxide or calcium oxide powder, carrying out a hydrogenation reaction process on the neutralized methanol solution in the presence of a Pd/C catalyst and an inhibitor, filtering the reaction product, and carrying out a salt formation reaction process on the filtrate and a sulfonyl salicylate methanol solution to obtain the doxycycline hydrochloride intermediate hydride. The preparation method is free of p-toluenesulfonic acid, has simple processes, can be operated easily and greatly reduces a production cost.

Description

technical field [0001] The application relates to the field of chemical synthesis of doxycycline hydrochloride, in particular to a preparation process of a doxycycline hydrochloride intermediate hydride. Background technique [0002] At present, the main process for the preparation of doxycycline hydrochloride is to use oxytetracycline as the starting raw material, and then undergo processes such as chlorination, dehydration, hydrogenation, conversion, and salt formation. Oxytetracycline chloride is dehydrated and salted with p-toluenesulfonic acid to form anhydrous 11α-chloro-4-(dimethylamino)-3,5,10,12α-tetrahydroxy-1,11,12-tri Oxo-1,4,4α,5,5α,6,11,11α,12,12α-decahydro-2-tetracenecarboxamide p-toluenesulfonate. After catalytic hydrogenation of the dehydrated product with Pd / C and auxiliary materials in an ethanol solvent, it is salified with sulfosalicylic acid to prepare 6α-methyl-4-(dimethylamino)-3,5,10,12,12α- Pentahydroxy-1,11-dioxo-1,4,4α,5,5α,6,11,12α-octahydro-2-...

Claims

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Application Information

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IPC IPC(8): C07C231/12C07C237/26C07C303/32C07C309/60
CPCC07C231/12C07C303/32C07C237/26C07C309/60
Inventor 黄业军
Owner 昆山华苏生物科技有限公司
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