CN102603774B - Addition technology for tetramisole hydrochloride - Google Patents

Addition technology for tetramisole hydrochloride Download PDF

Info

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
Authority
CN
China
Prior art keywords
addition
temperature
mass
kettle
technology
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201210028915.4A
Other languages
Chinese (zh)
Other versions
CN102603774A (en
Inventor
江耀田
杨劲松
冯进
盛海涛
陈虹
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CHANGZHOU YABANG-QH PHARMACHEM Co.,Ltd.
Inner Mongolia Qihui Pharmaceutical Co., Ltd
LIANYUNGANG YAHUI PHARMACHEM Co.,Ltd.
Original Assignee
NANTONG HAISHENG PHARMACEUTICAL CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by NANTONG HAISHENG PHARMACEUTICAL CO Ltd filed Critical NANTONG HAISHENG PHARMACEUTICAL CO Ltd
Priority to CN201210028915.4A priority Critical patent/CN102603774B/en
Publication of CN102603774A publication Critical patent/CN102603774A/en
Application granted granted Critical
Publication of CN102603774B publication Critical patent/CN102603774B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

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

Applications Claiming Priority (1)

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

Publications (2)

Publication Number Publication Date
CN102603774A CN102603774A (en) 2012-07-25
CN102603774B true CN102603774B (en) 2014-03-26

Family

ID=46521602

Family Applications (1)

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

Country Status (1)

Country Link
CN (1) CN102603774B (en)

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.

Also Published As

Publication number Publication date
CN102603774A (en) 2012-07-25

Similar Documents

Publication Publication Date Title
CN102532329B (en) Preparation method of low-viscosity octenyl succinic anhydride modified starch
CN102775441B (en) Continuous production method of glyphosate synthetic liquid
CN102558572B (en) Method for preparing xylogen acetylated derivative in ionic liquid solvent
CN104356365B (en) The production method of acid fiber by polylactic
CN103012167A (en) Preparation method of ambroxol hydrochloride
CN102181027B (en) Melamine formaldehyde resin modified by biomass materials and preparation method thereof
CN102603774B (en) Addition technology for tetramisole hydrochloride
CN101462980B (en) Industrial production method of 2,6-difluorobenzamide
CN103804173A (en) Fermentation organic acid refining method
CN103664835A (en) Preparation method of biological plasticizing agent epoxidized fatty acid methyl ester
CN102816333B (en) Preparation method of high-concentration PVA (polyvinyl alcohol) solution
Yuan et al. Engineering an industrial Saccharomyces cerevisiae strain with the inulinase gene for more efficient ethanol production from Jerusalem artichoke tubers
CN104388469A (en) Production method of biogas
CN102329249A (en) Method for chemically synthesizing guanidinopropionic acid
CN104447576A (en) Method for preparing 5-fluorouracil
CN104370830A (en) Synthetic method of 5-trifluoromethyl uracil
CN106810502A (en) A kind of preparation method of azoxystrobin intermediate
CN103467324B (en) Preparation method of N, N-dimethylglycine for industrial production
CN103387519B (en) Preparation method for 4-hydroxybenzyl cyanide
CN107868054A (en) A kind of preparation method of azoxystrobin intermediate
CN102382000A (en) Production method of D- para hydroxybenzene glycine
CN101759630A (en) Method for synthesizing N-benzyl-4-methyl-3-piperidone
CN100999478A (en) Process of preparing serine
CN101555499A (en) Technique for preparing 2-keto-D-gluconic acid by fermentation of corn starch
CN103664765A (en) Preparation method of 2-amino-3-bromopyridine

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20201027

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.