CN102603774B - Addition technology for tetramisole hydrochloride - Google Patents

Addition technology for tetramisole hydrochloride Download PDF

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Publication number
CN102603774B
CN102603774B CN201210028915.4A CN201210028915A CN102603774B CN 102603774 B CN102603774 B CN 102603774B CN 201210028915 A CN201210028915 A CN 201210028915A CN 102603774 B CN102603774 B CN 102603774B
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addition
temperature
mass
kettle
technology
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CN102603774A (en
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江耀田
杨劲松
冯进
盛海涛
陈虹
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CHANGZHOU YABANG-QH PHARMACHEM Co.,Ltd.
Inner Mongolia Qihui Pharmaceutical Co., Ltd
LIANYUNGANG YAHUI PHARMACHEM Co.,Ltd.
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NANTONG HAISHENG PHARMACEUTICAL CO Ltd
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Abstract

The invention discloses an addition technology for preparing tetramisole hydrochloride. The technology is characterized in that the technology comprises the following steps: weighing 230-240 parts by mass of styrene oxide with the mass concentration of 96-99%, pumping styrene oxide into a metering tank, weighing 695-705 parts by mass of ethanolamine with the mass concentration of 96-99%, pumping ethanolamine into an addition kettle, adding 4-6 parts by mass of sodium hydrogen carbonate to the addition kettle, starting stirring, heating until the temperature in the addition kettle is 58-60DEG C, adding styrene oxide to the addition kettle from the metering tank drop by drop, maintaining the temperature of a reaction liquid in the addition kettle at 58-60DEG C, adjusting the temperature after ending the 3-3.5h styrene oxide addition to make the temperature of the reaction liquid in the addition kettle rise to 61-63DEG C, ending an addition reaction after maintaining the temperature for 120-130min, and discharging the obtained material. The technology of the invention, which has the advantages of yield improvement, and reduction of the raw material consumption and the production cost of an enterprise, plays an effect in energy saving, emission reduction and environmental protection.

Description

A kind of additive process of preparing in tetramisole hydrochloride process
Technical field
The present invention relates to a kind of additive process of preparing in tetramisole hydrochloride process.
Background technology
Tetramisole hydrochloride is a kind of white crystalline powder, odorless, and bitter band is puckery.Soluble in water, methyl alcohol, be slightly dissolved in ethanol, and the atomic chloroform that is dissolved in, is insoluble to acetone.Its main application is as R-12564 intermediate, anthelmintic, vermifuge.Be used for roundworm, angle worm and retrofection.Current, the chemical products output such as the medicine of China, dyestuff continue steady-state growth always, and then drive the demand of tetramisole hydrochloride also to continue steady-state growth, and intermediate market demand further expands.The additive process that tetramisole hydrochloride is produced in existing employing Styrene oxide 98min., thanomin addition reaction does not add any catalyzer, causes the danger low, that produce of whole process recovery ratio many.Therefore, should provide a kind of new technical scheme to address the above problem.
Summary of the invention
The object of the invention is: for above-mentioned deficiency, provide the additive process of the tetramisole hydrochloride that a kind of product yield is high, Hazardous wastes generation is low, environmentally friendly, raw material consumption is low, production cost is few.
For achieving the above object, the technical solution used in the present invention is: a kind of additive process of preparing in tetramisole hydrochloride process, comprise the steps: to take the Styryl oxide that 230-240 mass parts mass concentrations are 96-99%, Styryl oxide is pumped in test tank, then take the thanomin that 695-705 mass parts mass concentrations are 96-99%, thanomin is pumped in addition still, again to the sodium bicarbonate that drops into 4-6 mass parts in addition still, open and stir, and heating, make addition temperature in the kettle be increased to 58-60 ℃, then from test tank, in addition still, drip Styryl oxide, control reacting liquid temperature in addition still and remain on 58-60 ℃, after 3-3.5h, Styryl oxide adds complete, regulate temperature, make reacting liquid temperature in addition still be increased to 61-63 ℃, after insulation 120-130min, addition reaction finishes, blowing.
A kind of additive process of preparing in tetramisole hydrochloride process of the present invention, take existing starting material Styryl oxide, thanomin is raw material, using sodium bicarbonate as catalyzer, organic raw material is reacted in suitable reaction system, reduce the generation of isomer in reaction process, thereby raising product yield, has simultaneously also reduced the generation of the Hazardous wastess such as resin in reaction process, environmentally friendly.
Advantage of the present invention is: the technique that the present invention adopts has improved yield, has reduced the production cost of raw material consumption and enterprise, has improved enterprise competitiveness, filled up again domestic blank simultaneously, has played the effect of energy-saving and emission-reduction, protection of the environment.
Embodiment
Embodiment 1
A kind of additive process of preparing in tetramisole hydrochloride process, comprise the steps: to take the Styryl oxide that 230 mass parts mass concentrations are 96%, Styryl oxide is pumped in test tank, then take the thanomin that 695 mass parts mass concentrations are 96%, thanomin is pumped in addition still, again to the sodium bicarbonate that drops into 4 mass parts in addition still, open and stir, and heating, make addition temperature in the kettle be increased to 58 ℃, then from test tank, in addition still, drip Styryl oxide, control reacting liquid temperature in addition still and remain on 58 ℃, after 3h, Styryl oxide adds complete, regulate temperature, make reacting liquid temperature in addition still be increased to 61 ℃, after insulation 120min, addition reaction finishes, blowing.
Embodiment 2
A kind of additive process of preparing in tetramisole hydrochloride process, comprise the steps: to take the Styryl oxide that 235 mass parts mass concentrations are 98%, Styryl oxide is pumped in test tank, then take the thanomin that 700 mass parts mass concentrations are 98%, thanomin is pumped in addition still, again to the sodium bicarbonate that drops into 5 mass parts in addition still, open and stir, and heating, make addition temperature in the kettle be increased to 59 ℃, then from test tank, in addition still, drip Styryl oxide, control reacting liquid temperature in addition still and remain on 59 ℃, after 200min, Styryl oxide adds complete, regulate temperature, make reacting liquid temperature in addition still be increased to 62 ℃, after insulation 125min, addition reaction finishes, blowing.
Embodiment 3
A kind of additive process of preparing in tetramisole hydrochloride process, comprise the steps: to take the Styryl oxide that 240 mass parts mass concentrations are 99%, Styryl oxide is pumped in test tank, then take 705 mass concentrations and be the thanomin of 99% mass parts, thanomin is pumped in addition still, again to the sodium bicarbonate that drops into 6 mass parts in addition still, open and stir, and heating, make addition temperature in the kettle be increased to 60 ℃, then from test tank, in addition still, drip Styryl oxide, control reacting liquid temperature in addition still and remain on 60 ℃, after 3.5h, Styryl oxide adds complete, regulate temperature, make reacting liquid temperature in addition still be increased to 63 ℃, after insulation 130min, addition reaction finishes, blowing.

Claims (1)

1. an additive process of preparing in tetramisole hydrochloride process, it is characterized in that comprising the steps: to take the Styryl oxide that 230-240 mass parts mass concentrations are 96-99%, by in Styryl oxide suction test tank, then the thanomin that the mass concentration that takes 695-705 mass parts is 96-99%, thanomin is pumped in addition still, again to the sodium bicarbonate that drops into 4-6 mass parts in addition still, open and stir, and heating, make addition temperature in the kettle be increased to 58-60 ℃, then from test tank, in addition still, drip Styryl oxide, control reacting liquid temperature in addition still and remain on 58-60 ℃, after 3-3.5h, Styryl oxide adds complete, regulate temperature, make reacting liquid temperature in addition still be increased to 61-63 ℃, after insulation 120-130min, addition reaction finishes, blowing.
CN201210028915.4A 2012-02-10 2012-02-10 Addition technology for tetramisole hydrochloride Active CN102603774B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210028915.4A CN102603774B (en) 2012-02-10 2012-02-10 Addition technology for tetramisole hydrochloride

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CN201210028915.4A CN102603774B (en) 2012-02-10 2012-02-10 Addition technology for tetramisole hydrochloride

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CN102603774B true CN102603774B (en) 2014-03-26

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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103242347B (en) * 2013-05-20 2015-04-08 黑龙江大学 Preparation method of tetramisole hydrochloride

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3855234A (en) * 1971-07-09 1974-12-17 Ici Ltd Manufacture of tetramisole
US4107170A (en) * 1975-10-29 1978-08-15 American Cyanamid Company Method of preparing dl 6-phenyl-2,3,5,6-tetrahydroimidazo-[2,1-b]thiazole and acid addition salts thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3855234A (en) * 1971-07-09 1974-12-17 Ici Ltd Manufacture of tetramisole
US4107170A (en) * 1975-10-29 1978-08-15 American Cyanamid Company Method of preparing dl 6-phenyl-2,3,5,6-tetrahydroimidazo-[2,1-b]thiazole and acid addition salts thereof

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
氧化苯乙烯-乙醇胺加成法合成四咪唑中间试验;陈玉书等;《医药工业》;19791231(第11期);第11-14页 *
盐酸四咪唑合成工艺及后处理技术的研究;郑博等;《山东医药工业》;19961231;第15卷(第2期);第1-2页 *
郑博等.盐酸四咪唑合成工艺及后处理技术的研究.《山东医药工业》.1996,第15卷(第2期),第1-2页.
陈玉书等.氧化苯乙烯-乙醇胺加成法合成四咪唑中间试验.《医药工业》.1979,(第11期),第11-14页.

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Address after: No.18, Jinlong Road, Chunjiang Town, Xinbei District, Changzhou City, Jiangsu Province, 213000

Patentee after: CHANGZHOU YABANG-QH PHARMACHEM Co.,Ltd.

Patentee after: Inner Mongolia Qihui Pharmaceutical Co., Ltd

Patentee after: LIANYUNGANG YAHUI PHARMACHEM Co.,Ltd.

Address before: 226100, Jiangsu, Nantong Haimen Ling industrial concentration zone

Patentee before: NANTONG HAISHENG PHARMACEUTICAL Co.,Ltd.