CN101643419A - Method for preparing o-nitroanisole - Google Patents
Method for preparing o-nitroanisole Download PDFInfo
- Publication number
- CN101643419A CN101643419A CN200810139122A CN200810139122A CN101643419A CN 101643419 A CN101643419 A CN 101643419A CN 200810139122 A CN200810139122 A CN 200810139122A CN 200810139122 A CN200810139122 A CN 200810139122A CN 101643419 A CN101643419 A CN 101643419A
- Authority
- CN
- China
- Prior art keywords
- methyl ether
- nitrophenyl methyl
- nitroanisole
- organic solvent
- nitrophenyl
- 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
- CFBYEGUGFPZCNF-UHFFFAOYSA-N 2-nitroanisole Chemical compound COC1=CC=CC=C1[N+]([O-])=O CFBYEGUGFPZCNF-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title abstract 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 6
- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000006198 methoxylation reaction Methods 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 238000004821 distillation Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- JRBJSXQPQWSCCF-UHFFFAOYSA-N 3,3'-Dimethoxybenzidine Chemical compound C1=C(N)C(OC)=CC(C=2C=C(OC)C(N)=CC=2)=C1 JRBJSXQPQWSCCF-UHFFFAOYSA-N 0.000 description 1
- DSBIJCMXAIKKKI-UHFFFAOYSA-N 5-nitro-o-toluidine Chemical compound CC1=CC=C([N+]([O-])=O)C=C1N DSBIJCMXAIKKKI-UHFFFAOYSA-N 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VMPITZXILSNTON-UHFFFAOYSA-N o-anisidine Chemical compound COC1=CC=CC=C1N VMPITZXILSNTON-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing o-nitroanisole. The method comprises the following steps: performing a methoxylation reaction in organic solvent and basic state; and collecting the o-nitroanisole from a reactant by adopting a conventional method, wherein the molar yield of the finished product reaches over 90 percent. The method has reasonable process route; and the finished productprepared by adopting the method has higher yield and purity, thus has larger industrial prospect.
Description
Technical field
The present invention relates to a kind of preparation method of o-Nitrophenyl methyl ether.
Background technology
O-Nitrophenyl methyl ether is a kind of important dyestuff, medicine intermediate, is mainly used in production Ortho Anisidine and dianisidine, Fast Scarlet G B etc.Current preparation o-Nitrophenyl methyl ether generally forms by methoxylation.But exist sometimes processing step not too rationally, the inaccurate problem of processing parameter, cause that prepared product yield is not high, cost is bigger, and raw material can not be fully utilized.
Summary of the invention
For solving the problem of above existence, the invention provides a kind of preparation method of o-Nitrophenyl methyl ether, its technical scheme of taking is:
O-Nitrophenyl methyl ether is prepared from by following steps:
1) in stainless steel autoclave, adds o-Nitrochlorobenzene, organic solvent, 30% sodium hydroxide solution, behind the good seal, pressure-controlling is at 0.1～1Mpa, temperature is controlled at 30～60 ℃, reacted 3～5 hours, generated o-Nitrophenyl methyl ether in 1 hour 80～100 ℃ of insulations again, the filtrate layering, washing, distillation are the o-Nitrophenyl methyl ether finished product.
Organic solvent is the methyl alcohol that dissolves each other with o-Nitrochlorobenzene.
Embodiment
Below in conjunction with embodiment the present invention is elaborated:
In stainless steel autoclave, add o-Nitrochlorobenzene 100g, methyl alcohol 250ml, sodium hydroxide 32g, good seal, pressure-controlling is at 0.1～1Mpa, temperature is controlled at 30～60 ℃, reacts 3～5 hours, generates o-Nitrophenyl methyl ether in 10 hours 80～100 ℃ of insulations then, the filtrate layering, with methyl alcohol 100ml washing, be o-Nitrophenyl methyl ether after the distillation, the whole recovery sets of solvent for use are used.It is 95% that o-Nitrophenyl methyl ether calculates o-Nitrophenyl methyl ether mole rate according to liquid-phase chromatographic analysis.
Claims (2)
1, a kind of preparation method of o-Nitrophenyl methyl ether is characterized in that being prepared from by following steps:
In stainless steel autoclave, add o-Nitrochlorobenzene, organic solvent, sodium hydroxide solution, pressure-controlling is at 0.2～1Mpa, and temperature is controlled at 30～60 ℃, reacts 3～5 hours, be incubated then about 10 hours, by separating, wash, distill the generation o-Nitrophenyl methyl ether.
2, according to the preparation method of the described o-Nitrophenyl methyl ether of claim 1, it is characterized in that: described organic solvent for the methyl alcohol of o-Nitrophenyl methyl ether.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810139122A CN101643419A (en) | 2008-08-08 | 2008-08-08 | Method for preparing o-nitroanisole |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200810139122A CN101643419A (en) | 2008-08-08 | 2008-08-08 | Method for preparing o-nitroanisole |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101643419A true CN101643419A (en) | 2010-02-10 |
Family
ID=41655508
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200810139122A Pending CN101643419A (en) | 2008-08-08 | 2008-08-08 | Method for preparing o-nitroanisole |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101643419A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320978A (en) * | 2011-09-22 | 2012-01-18 | 江苏康恒化工有限公司 | Preparation method of anhydrous system o-nitroanisole |
| CN102344372A (en) * | 2011-07-29 | 2012-02-08 | 江苏力达宁化工有限公司 | Synthetic method of o-nitrophenol and o-nitroanisole |
| CN105503610A (en) * | 2014-09-23 | 2016-04-20 | 中国石油化工股份有限公司 | Method for preparing o-nitro anisole by using micro-channel reaction apparatus |
-
2008
- 2008-08-08 CN CN200810139122A patent/CN101643419A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344372A (en) * | 2011-07-29 | 2012-02-08 | 江苏力达宁化工有限公司 | Synthetic method of o-nitrophenol and o-nitroanisole |
| CN102320978A (en) * | 2011-09-22 | 2012-01-18 | 江苏康恒化工有限公司 | Preparation method of anhydrous system o-nitroanisole |
| CN105503610A (en) * | 2014-09-23 | 2016-04-20 | 中国石油化工股份有限公司 | Method for preparing o-nitro anisole by using micro-channel reaction apparatus |
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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 |
Open date: 20100210 |