CN102311362A - Method for preparing ethyl hydrazinoacetate hydrochloride - Google Patents
Method for preparing ethyl hydrazinoacetate hydrochloride Download PDFInfo
- Publication number
- CN102311362A CN102311362A CN2010102194785A CN201010219478A CN102311362A CN 102311362 A CN102311362 A CN 102311362A CN 2010102194785 A CN2010102194785 A CN 2010102194785A CN 201010219478 A CN201010219478 A CN 201010219478A CN 102311362 A CN102311362 A CN 102311362A
- Authority
- CN
- China
- Prior art keywords
- hydrazine
- ethyl acetate
- sodium
- acetate hydrochloride
- preparation
- 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.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for preparing ethyl hydrazinoacetate hydrochloride. The method comprises the following steps of: mixing and heating chloroacetic acid, hydrazine hydrate and alkali, and reacting at the temperature of between 0 and 25 DEG C to obtain a product sodium hydrazinoacetate; concentrating under reduced pressure, separating water, filtering, adding absolute ethanol, and performing esterification reaction by drying hydrogen chloride to obtain ethyl hydrazinoacetate hydrochloride and sodium chloride; and filtering to obtain a filter cake and filtrate, cooling the filtrate, crystallizing and separating to obtain the ethyl hydrazinoacetate hydrochloride and the filtrate, drying the ethyl hydrazinoacetate hydrochloride to obtain a product, distilling the filtrate to obtain diluted ethanol and leftover materials, and dehydrating the diluted ethanol to obtain the absolute ethanol. The method has the advantages of reducing the consumption of raw materials, improving production efficiency and reducing production cost along with good safety performance and is easy to operate.
Description
Technical field
The present invention relates to a kind of preparation method of hydrazine ethyl acetate hydrochloride.
Background technology
Chaste tree guanidine-acetic acid carbethoxy hydrochloride is a kind of important organic synthesis intermediate, can be used as the midbody of synthetic drugs especially, has very to use widely.
Domestic hydrazine ethyl acetate hydrochloride a large amount of waste residues, cinder can occur in process of production at present; Contaminate environment, rate of utilization is low, and the product that circulates on the China market is basically all from Europe; Price comparison is expensive, if all poor from external import social benefit and economic benefit.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of hydrazine ethyl acetate hydrochloride.
The technical scheme that the present invention adopts is:
The preparation method of hydrazine ethyl acetate hydrochloride may further comprise the steps:
With Mono Chloro Acetic Acid, sodium hydroxide and Hydrazine Hydrate 80 Hybrid Heating, isothermal reaction obtains product hydrazine sodium acetate; After reducing pressure, concentrate, divide water, filtration, add absolute ethyl alcohol and carry out esterification, obtain hydrazine acetate, carbethoxy hydrochloride and sodium-chlor through dry hydrogen chloride; Through filtering filter cake and filtrating; Filtrating obtains hydrazine ethyl acetate hydrochloride and filtrating through cooling, crystallization, separation, the hydrazine ethyl acetate hydrochloride advance to dry product; Filtrating obtains light ethanol and pin material through distillation, and light ethanol obtains absolute ethyl alcohol through dehydration.
Said alkali is a kind of in yellow soda ash, sodium hydroxide, Pottasium Hydroxide or the sodium ethylate
Said Mono Chloro Acetic Acid: alkali: the mol ratio of Hydrazine Hydrate 80 is 1-1.5: 1: 2-2.2.
Said Hydrazine Hydrate 80 content is 40-90%.
Said filter cake is a sodium-chlor, filtrates to be the ethanolic soln of hydrazine ethyl acetate hydrochloride.
Said what is said or talked about alcoholic acid content is 10%-15%H
2O.
Advantage of the present invention is: reduce consumption of raw materials, enhance productivity, reduce production costs, simple to operate, safety performance is good.
Embodiment
Through embodiment the present invention is described further below.
Step of the present invention comprises the steps:
Reaction formula of the present invention is following:
CLCH
2COOH+NH
2NH
2+NaOH→NH
2NHCH
2COONa+NaCL+H
2O
NH
2NHCH
2COONa+HCL+C
2H
2OH→NH
2NHCH
2COO?C
2H
5.?HCL+NaCL+H
2O
Embodiment 1
The hydrazine ethyl acetate hydrochloride at first mixed 1 hour with the sodium hydroxide heating with 90% Hydrazine Hydrate 80 as starting raw material from Mono Chloro Acetic Acid; Make the hydrazine sodium acetate 25 ℃ of reactions then, have sodium-chlor and water to generate in this process, before getting into the reaction of second step, must water be removed; Then directly and hydrogenchloride and ethanol synthesis with the mixture of hydrazine sodium acetate and sodium-chlor; The hydrazine sodium acetate generates the hydrazine ethyl acetate hydrochloride in this process, and reaction utilizes hydrazine ethyl acetate hydrochloride, the sodium-chlor difference of solubleness in hot ethanol to separate after ending; Filtrating is the ethanolic soln of hydrazine ethyl acetate hydrochloride, and filter cake is a sub product sodium-chlor.The ethanolic soln cooling of heat can be obtained a large amount of crystallizations, and centrifugal, oven dry obtains product, productive rate 98%.From the mother liquor of centrifugal gained, reclaiming the ethanol water cut is 15%, and the treated absolute ethyl alcohol that obtains can be used for next batch and feeds intake; When reclaiming solvent, there are the product and the unreacted raw material that are partially dissolved in the mother liquor to separate out, can be used for next batch equally and feed intake; Thereby make conversion of raw material improve, solvent consumption reduces, when having reduced production cost; Reduce discharging, accomplish qualified discharge.
Embodiment 2
The hydrazine ethyl acetate hydrochloride at first mixed 0.5 hour with the sodium hydroxide heating with 40% Hydrazine Hydrate 80 as starting raw material from Mono Chloro Acetic Acid; Make the hydrazine sodium acetate 15 ℃ of reactions then, have sodium-chlor and water to generate in this process, before getting into the reaction of second step, must water be removed; Then directly and hydrogenchloride and ethanol synthesis with the mixture of hydrazine sodium acetate and sodium-chlor; The hydrazine sodium acetate generates the hydrazine ethyl acetate hydrochloride in this process, and reaction utilizes hydrazine ethyl acetate hydrochloride, the sodium-chlor difference of solubleness in hot ethanol to separate after ending; Filtrating is the ethanolic soln of hydrazine ethyl acetate hydrochloride, and filter cake is a sub product sodium-chlor.The ethanolic soln cooling of heat can be obtained a large amount of crystallizations, and centrifugal, oven dry obtains product, productive rate 88%.From the mother liquor of centrifugal gained, reclaiming the ethanol water cut is 12%, and the treated absolute ethyl alcohol that obtains can be used for next batch and feeds intake; When reclaiming solvent, there are the product and the unreacted raw material that are partially dissolved in the mother liquor to separate out, can be used for next batch equally and feed intake; Thereby make conversion of raw material improve, solvent consumption reduces, when having reduced production cost; Reduce discharging, accomplish qualified discharge.
Embodiment 3
The hydrazine ethyl acetate hydrochloride at first mixed 0.2 hour with the sodium hydroxide heating with 60% Hydrazine Hydrate 80 as starting raw material from Mono Chloro Acetic Acid; Make the hydrazine sodium acetate 5 ℃ of reactions then, have sodium-chlor and water to generate in this process, before getting into the reaction of second step, must water be removed; Then directly and hydrogenchloride and ethanol synthesis with the mixture of hydrazine sodium acetate and sodium-chlor; The hydrazine sodium acetate generates the hydrazine ethyl acetate hydrochloride in this process, and reaction utilizes hydrazine ethyl acetate hydrochloride, the sodium-chlor difference of solubleness in hot ethanol to separate after ending; Filtrating is the ethanolic soln of hydrazine ethyl acetate hydrochloride, and filter cake is a sub product sodium-chlor.The ethanolic soln cooling of heat can be obtained a large amount of crystallizations, and centrifugal, oven dry obtains product, productive rate 78%.From the mother liquor of centrifugal gained, reclaiming the ethanol water cut is 10%, and the treated absolute ethyl alcohol that obtains can be used for next batch and feeds intake; When reclaiming solvent, there are the product and the unreacted raw material that are partially dissolved in the mother liquor to separate out, can be used for next batch equally and feed intake; Thereby make conversion of raw material improve, solvent consumption reduces, when having reduced production cost; Reduce discharging, accomplish qualified discharge.
Claims (6)
1. the preparation method of hydrazine ethyl acetate hydrochloride may further comprise the steps:
With Mono Chloro Acetic Acid, Hydrazine Hydrate 80 and alkali Hybrid Heating, under 0-25 ℃ of reaction, obtain product hydrazine sodium acetate, decompression, concentrate, divide water, filter after; Add absolute ethyl alcohol and carry out esterification through dry hydrogen chloride; Obtain hydrazine acetate, carbethoxy hydrochloride and sodium-chlor, through filtering filter cake and filtrating, filtrating is through cooling, crystallization, separation; Obtain hydrazine ethyl acetate hydrochloride and filtrating; The hydrazine ethyl acetate hydrochloride advance to dry product, filtrating through the distillation obtain light ethanol and pin material, light ethanol obtains absolute ethyl alcohol through dehydration.
2. the preparation method of hydrazine ethyl acetate hydrochloride according to claim 1 is characterized in that said alkali is a kind of in yellow soda ash, sodium hydroxide, Pottasium Hydroxide or the sodium ethylate.
3. the preparation method of hydrazine ethyl acetate hydrochloride according to claim 1 is characterized in that said Mono Chloro Acetic Acid: alkali: the mol ratio of Hydrazine Hydrate 80 is 1-1.5: 1: 2-2.2.
4. the preparation method of hydrazine ethyl acetate hydrochloride according to claim 1 is characterized in that said Hydrazine Hydrate 80 content is 40-90%.
5. the preparation method of hydrazine ethyl acetate hydrochloride according to claim 1 is characterized in that said filter cake is a sodium-chlor, and filtrating is the ethanolic soln of hydrazine ethyl acetate hydrochloride.
6. the preparation method of hydrazine ethyl acetate hydrochloride according to claim 1 is characterized in that said what is said or talked about alcoholic acid content is 10%-15%H
2O.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102194785A CN102311362A (en) | 2010-06-30 | 2010-06-30 | Method for preparing ethyl hydrazinoacetate hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102194785A CN102311362A (en) | 2010-06-30 | 2010-06-30 | Method for preparing ethyl hydrazinoacetate hydrochloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102311362A true CN102311362A (en) | 2012-01-11 |
Family
ID=45424969
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102194785A Pending CN102311362A (en) | 2010-06-30 | 2010-06-30 | Method for preparing ethyl hydrazinoacetate hydrochloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102311362A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111371A (en) * | 2018-09-27 | 2019-01-01 | 郑州盖科科技有限公司 | A kind of preparation method of diazanyl ethyl acetate hydrochloride |
| CN109134296A (en) * | 2018-09-27 | 2019-01-04 | 郑州盖科科技有限公司 | A kind of synthetic method of diazanyl ethyl acetate hydrochloride |
-
2010
- 2010-06-30 CN CN2010102194785A patent/CN102311362A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109111371A (en) * | 2018-09-27 | 2019-01-01 | 郑州盖科科技有限公司 | A kind of preparation method of diazanyl ethyl acetate hydrochloride |
| CN109134296A (en) * | 2018-09-27 | 2019-01-04 | 郑州盖科科技有限公司 | A kind of synthetic method of diazanyl ethyl acetate hydrochloride |
| CN109111371B (en) * | 2018-09-27 | 2021-08-06 | 江西万里药业有限公司 | Preparation method of hydrazino ethyl acetate hydrochloride |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102617542B (en) | Method for preparing and purifying olmesartan intermediate | |
| CN102627608B (en) | Preparation method for analgesic and antipyretic drug-analgin | |
| CN103724279B (en) | One step to form the loop prepares the convenient synthetic method of 2-methyl-4-amino-5-amino methylpyrimidine | |
| US20120095261A1 (en) | Process for preparation of alpha-ketoglutaric acid | |
| CN101863784A (en) | Methods for preparing and extracting betaine and betaine hydrochloride | |
| CN103396318B (en) | Synthetic process for 2,4-dinitroanisole | |
| CN102311394B (en) | Preparation method for 5-ethyl-5-phenyl barbituric acid | |
| CN111393331B (en) | Preparation method of glycocyamine | |
| CN102311362A (en) | Method for preparing ethyl hydrazinoacetate hydrochloride | |
| CN101781264B (en) | Production method of 1-methyl-5-mercapto-1,2,3,4-tetrazole | |
| CN101693685A (en) | Method for preparing 4-hydroxylethylpyrrolidone-2-acetamide | |
| CN101875640B (en) | Method for preparing pyrazinecarboxylic acid in ionic liquid | |
| CN102617461A (en) | Novel method for refining aripiprazole | |
| CN102675243A (en) | Process for synthesizing intermediate of (S)-2,6-diamino-4,5,6,7-tetralinbenzothiazole of anti-parkinson drug | |
| CN102382050A (en) | Preparation method of substituted 1, 2, 3 and 4- tetrahydroquinoline -4-one hydrochloride | |
| CN101723842B (en) | Method for preparing ethylene diamine tetraacetic acid (EDTA) disodium salt | |
| CN102146022B (en) | Method for preparing 3-chlorine-5-bromophenol | |
| CN103951596A (en) | Preparation method of medicinal D, L-alpha-hydroxymethionine calcium | |
| CN103360235A (en) | Preparation method of barium acetate | |
| CN102659579A (en) | preparation method of p-chlorine methyl cinnamate | |
| CN101823986A (en) | Preparation method for tert-butyl carbazate | |
| CN102690312A (en) | Purification method for lanolin cholesterol | |
| CN101823982A (en) | Method for preparing hydrazine ethyl acetate hydrochloride | |
| CN102633624B (en) | Method for preparing methylcinnamic acid | |
| CN105017029A (en) | Preparation method of p-bromoaniline |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120111 |