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Preparation method of acetamidine hydrochloride

A technology of acetamidine hydrochloride and acetonitrile, applied in the field of preparation of acetamidine hydrochloride, can solve the problems of low production process yield and high production cost

Pending Publication Date: 2020-06-12
唐山威格化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The production process yield of producing acetamidine hydrochloride is low at present, and production cost is high

Method used

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  • Preparation method of acetamidine hydrochloride

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Embodiment 1

[0021] The embodiment of the present invention discloses a kind of preparation method of acetamidine hydrochloride, as shown in the figure, comprises the following steps:

[0022] a. Hydrogen chloride is passed into the kettle that has the concentrated sulfuric acid to dry, then forms acid methanol with methanol, and the concentration of acid methanol is 46% (w / w);

[0023] b. Put the acid methanol into the reaction kettle, slowly add acetonitrile dropwise through the metering tank, so that the temperature is controlled at 9°C; after adding the acetonitrile, keep it at about 20°C for 5 hours to synthesize acetamidine;

[0024] c. After the ethyleneamidine synthesis is completed, open the reactor jacket brine, and add a certain amount of methanol to make the temperature of the material drop to -5°C, then add ammonia methanol in the reactor, and the concentration of ammonia methanol is 17% (w / w ), add slowly in the early stage to control the temperature at 0~-5°C, when 1 / 3 of th...

Embodiment 2

[0027] Embodiments of the present invention disclose a kind of preparation method of acetamidine hydrochloride, comprising the following steps:

[0028] a. Hydrogen chloride is passed into the still that has the concentrated sulfuric acid to dry, then forms acid methanol with methanol, and the concentration of acid methanol is 46.8% (w / w);

[0029] b. Put the acid methanol into the reaction kettle, slowly add acetonitrile dropwise through the metering tank, so that the temperature is controlled at 10°C; after adding the acetonitrile, keep it at about 25°C for 6 hours to synthesize acetamidine;

[0030] c. After the ethyleneamidine synthesis is completed, open the reactor jacket brine, and add a certain amount of methanol to make the temperature of the material drop to -5°C, then add ammonia methanol in the reactor, and the concentration of ammonia methanol is 16% (w / w ), add slowly in the early stage to control the temperature at 0~-5°C, when 1 / 3 of the amount is added, when p...

Embodiment 3

[0033] Embodiments of the present invention disclose a kind of preparation method of acetamidine hydrochloride, comprising the following steps:

[0034] a. Hydrogen chloride is passed into the kettle that has the concentrated sulfuric acid to dry, then forms acid methanol with methanol, and the concentration of acid methanol is 48% (w / w);

[0035] b. Put the acid methanol into the reaction kettle, slowly add acetonitrile dropwise through the metering tank, so that the temperature is controlled at 11°C; after adding the acetonitrile, keep it at about 28°C for 7 hours to synthesize acetamidine;

[0036] c. After the synthesis of ethyleneamidine is completed, open the reactor jacket brine, and add a certain amount of methanol to make the temperature of the material drop to -5 ° C, then add ammonia methanol in the reactor, and the concentration of ammonia methanol is 15% (w / w ), add slowly in the early stage to control the temperature at 0~-5°C, when 1 / 3 of the amount is added, wh...

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Abstract

The invention discloses a preparation method of acetamidine hydrochloride. The preparation method comprises the following steps: a. introducing hydrogen chloride into a kettle in which concentrated sulfuric acid is stored, drying, and forming acid methanol with methanol; b, adding acid methanol into the reaction kettle, slowly dropwise adding acetonitrile through a metering tank, and controlling the temperature to be 9-11 DEG C; after acetonitrile is added, performing heat preservation for 5-7 hours at the temperature of about 20-28 DEG C to synthesize acetamidine; c, adding aminomethanol intothe reaction kettle, slowly adding in the earlier stage to control the temperature to be 0--5 DEG C, and quickly adding aminomethanol until the pH value is 7-8 when the adding amount is 1 / 3 and the pH value is 4-5 so as to complete ammoniation reaction; and d, after the ammoniation reaction is finished, centrifuging ammonium chloride, distilling off methanol, and centrifuging to obtain an acetamidine hydrochloride finished product. According to the method, the material ratio and process control indexes are adjusted and optimized so that the product yield is obviously improved, the product quality is obviously superior to relevant national standards, in addition, the equipment production capacity is enlarged, the methanol consumption is reduced and the operation is safe and feasible.

Description

technical field [0001] The invention belongs to the technical field of chemical intermediates, in particular to a preparation method of acetamidine hydrochloride. Background technique [0002] Acetidine hydrochloride is white long-edged (or needle-like) crystals, industrial products are generally slightly yellow, acetamidine hydrochloride is easy to deliquescence, has a unique odor, soluble in water and ethanol, insoluble in ether and acetone, melting point 166 ~167°C and 177~178°C (two crystal forms). Acetidine hydrochloride is mainly used for the production of pharmaceutical vitamin B1, and can also be used as a basic raw material for organic synthesis, with a wide range of uses. The production process yield of producing acetamidine hydrochloride is low at present, and production cost is high. Contents of the invention [0003] Aiming at the technical problems existing in the prior art, the present invention provides a preparation method of acetamidine hydrochloride, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C257/14C07C257/06
CPCC07C257/14C07C257/06
Inventor 张晓航
Owner 唐山威格化学工业有限公司
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