CN102382011A - Preparation process of 4-nitrophenyl hydrazine hydrochloride - Google Patents
Preparation process of 4-nitrophenyl hydrazine hydrochloride Download PDFInfo
- Publication number
- CN102382011A CN102382011A CN201010270918XA CN201010270918A CN102382011A CN 102382011 A CN102382011 A CN 102382011A CN 201010270918X A CN201010270918X A CN 201010270918XA CN 201010270918 A CN201010270918 A CN 201010270918A CN 102382011 A CN102382011 A CN 102382011A
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- China
- Prior art keywords
- hydrazine hydrochloride
- nitrophenyl hydrazine
- reaction
- preparation process
- hydrochloride
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- 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.)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation process of 4-nitrophenyl hydrazine hydrochloride. Aminophenyl sulfonamide as an initial raw material and is subjected to a diazo reaction, a reducing reaction and hydrolysis to obtain p-nitrophenyl hydrazine hydrochloride, wherein sodium metabisulfite is used as the reducing agent in the reducing reaction; and the reducing reaction is carried out under the conditions that the temperature is 10-35DEG C and the pH value is 5-8. The p-nitrophenyl hydrazine hydrochloride product obtained by adopting the method has high purity and low production cost.
Description
Technical field
The invention belongs to the preparation method of organic chemical industry's product, particularly the preparation technology of nitrophenyl hydrazine hydrochloride.
Background technology
The paranitrophenylhydrazine hydrochloride is a kind of important midbody, especially a kind of medicine intermediate, and prior art is being raw material to sulfonamido aniline; Through diazotization reaction, S-WAT reduction, hydrolysis, the compound method of the paranitrophenylhydrazine hydrochloride for preparing; Long reaction time, production cost is high.
Summary of the invention
The problem that will solve required for the present invention provides the preparation technology of nitrophenyl hydrazine hydrochloride, and the paranitrophenylhydrazine hydrochloride product purity that is obtained by this method is high, and production cost is low.
The preparation technology of nitrophenyl hydrazine hydrochloride, to be starting raw material to sulfonamido aniline, through diazotization reaction, reduction reaction, hydrolysis prepare the paranitrophenylhydrazine hydrochloride, and at 5-55 ℃, pH carries out under the condition of 5-8.And Sodium Pyrosulfite can shorten the reaction times so greatly as reductive agent, and the product purity that obtains is high, and production cost is low.
Embodiment
In the 100ml flask, add sulfonamido aniline 3.5 grams, water 10ml, 10N hydrochloric acid 5ml, stirring and dissolving, be cooled to below 0 ℃ after, add sodium nitrite solution, 0-5 ℃ of reaction 5 minutes, filter and remove residue, diazonium salt solution.
Sodium Pyrosulfite 6.5 gram, water 25ml, 10N sodium hydroxide 5ml stirring and dissolving is made into the Sodium Pyrosulfite alkaline solution, be cooled to 10-20 ℃ after; Above-mentioned diazonium salt solution is added, and the adjusting pH value is 5-8, after 30 minutes, adds 10N hydrochloric acid 10ml 20-30 ℃ of reaction; Be heated to 90-105 ℃, react after 30 minutes, add activated carbon 0.1 gram; 10 ℃ of filtrations of filter and remove residue postcooling are purified, the dry product that gets.According to the size and the complexity of artwork, can before injection molding, increase netted reinforcing rib and body muscle on demand.The structure that moulding is complicated can be used the split mould, adopts secondary or injection molding repeatedly.
Claims (1)
1. the preparation technology of nitrophenyl hydrazine hydrochloride, to be starting raw material to sulfonamido aniline, through diazotization reaction, reduction reaction, hydrolysis prepare the paranitrophenylhydrazine hydrochloride, it is characterized in that: at 5-55 ℃, pH carries out under the condition of 5-8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010270918XA CN102382011A (en) | 2010-09-03 | 2010-09-03 | Preparation process of 4-nitrophenyl hydrazine hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010270918XA CN102382011A (en) | 2010-09-03 | 2010-09-03 | Preparation process of 4-nitrophenyl hydrazine hydrochloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102382011A true CN102382011A (en) | 2012-03-21 |
Family
ID=45821907
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010270918XA Pending CN102382011A (en) | 2010-09-03 | 2010-09-03 | Preparation process of 4-nitrophenyl hydrazine hydrochloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102382011A (en) |
-
2010
- 2010-09-03 CN CN201010270918XA patent/CN102382011A/en active Pending
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| DD01 | Delivery of document by public notice |
Addressee: Yuan Xuechong Document name: Notification of Passing Preliminary Examination of the Application for Invention |
|
| C06 | Publication | ||
| PB01 | Publication | ||
| DD01 | Delivery of document by public notice |
Addressee: Yuan Xuechong Document name: Notification of Publication of the Application for Invention |
|
| DD01 | Delivery of document by public notice |
Addressee: Yuan Xuechong Document name: Notification of before Expiration of Request of Examination as to Substance |
|
| DD01 | Delivery of document by public notice |
Addressee: Yuan Xuechong Document name: Notification that Application Deemed to be Withdrawn |
|
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120321 |