CN104610065B - A kind of 2, the preparation method of 2 '-dinitrobenzene dibenzyl - Google Patents
A kind of 2, the preparation method of 2 '-dinitrobenzene dibenzyl Download PDFInfo
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- CN104610065B CN104610065B CN201410594600.5A CN201410594600A CN104610065B CN 104610065 B CN104610065 B CN 104610065B CN 201410594600 A CN201410594600 A CN 201410594600A CN 104610065 B CN104610065 B CN 104610065B
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- dinitrobenzene
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Abstract
The present invention relates to a kind of methodology of organic synthesis, particularly relate to a kind of 2, the preparation method of 2 '-dinitrobenzene dibenzyl.The method is distributed to sodium methylate in paraffin oil, controls certain temperature of reaction, instills Ortho Nitro Toluene with methane amide simultaneously, then through operations such as insulation, hydrolysis, dealcoholysis, separation, washing, dryings, obtained 2,2 '-dinitrobenzene dibenzyl finished product, yield 82.5%.Feature of the present invention is an improvement technological process, improves the yield of target product, reduces production cost, decreases the discharge of pollutent simultaneously.
Description
Technical field
The present invention relates to a kind of 2, the preparation method of 2 '-dinitrobenzene dibenzyl, belongs to the field of chemical synthesis.
Background technology
Existing synthesis 2, the method for 2 '-dinitrobenzene dibenzyl is distributed in solvent sherwood oil by sodium methylate, controls certain temperature of reaction, instillation Ortho Nitro Toluene is with ethyl formate mixed solution, again through insulation, hydrolysis, be separated, washing, dry 2,2 '-dinitrobenzene dibenzyl, yield is about 75%.，
The method main drawback is: 1. sherwood oil is as low boil-off dose, and consume large, operating environment is poor; 2. this reaction is wayward, often there will be temperature and suddenly raises phenomenon, causes the danger of punching material; 3., when being separated, because low boil-off dose containing methyl alcohol, ethanol etc. in system, product solubleness in mother liquor can be made to increase, affect yield; 4. in the waste water that produces of reaction because of containing a large amount of alkali, nitro compounds, alcohol, be difficult to process further.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of process stabilizing, yield is high, and cost is low, pollutes few 2, the preparation method of 2 '-dinitrobenzene dibenzyl.
Present invention employs following technical scheme: in reactor, add sodium methylate and paraffin oil, control temperature 5 ~ 10 DEG C, instill Ortho Nitro Toluene with methane amide simultaneously, insulation obtained 2,2 '-dinitrobenzene dibenzyl reaction mixture, then through hydrolysis, dealcoholysis, separation, washing, dry product yield 82.5%.
Feature of the present invention is: 1. have employed paraffin oil is that raw material replaces sherwood oil, and paraffin oil has colourless, tasteless, nontoxic, Stability Analysis of Structures, boiling point high, relative sherwood oil, and solvent consumption greatly reduces, and operating environment is also greatly improved.2. methane amide replaces ethyl formate, and methane amide molecular weight is little on the one hand, and low price, can reduce raw materials cost; On the other hand, methane amide is more stable relative to ethyl formate structure, and reaction is milder, solves and easily rushes material problem.3. first remove alcohol before being separated, make product precipitation as much as possible, not only can improve yield, reclaimed methyl alcohol, and make waste component relatively simple, be convenient to processing and utilizing.
In a word: the present invention improves technological process, improve the yield of target product, reduce production cost, also reduce the pollution of whole production process to environment simultaneously.
Embodiment
Below in conjunction with specific embodiment, the present invention is made a detailed explanation.
Embodiment
In 500ml four-hole bottle, add sodium methylate 32.5g and paraffin oil 180g, stir, sodium methylate is distributed in paraffin oil.Control temperature is at 5 ~ 10 DEG C, and instill Ortho Nitro Toluene 80g and methane amide 13.7g, time for adding amounts to 2.5 hours simultaneously.Then be warmed up to 10 ~ 15 DEG C after 4 hours 5 ~ 10 DEG C of insulations and continue insulation 6 hours, condensation obtained 2,2 '-dinitrobenzene dibenzyl reaction mixture.In reaction solution, be added dropwise to 180g water (water is applied mechanically in available washing) again, maintain the temperature at 30 ~ 40 DEG C of hydrolysis one hour.Be hydrolyzed complete, heat up, steam except methyl alcohol, make temperature steam to 95 DEG C, amount to and reclaim methyl alcohol 25g (moisture 23.7%).After having taken off alcohol, reaction solution is as cold as 30 ~ 40 DEG C, suction filtration, mother liquor separates buck layer (182g altogether, alkali content 12.1%).Suction filtration gained filter cake again through washing, dry finished product 65.5g, content 98.5%, yield 82.5%.
Claims (9)
1. one kind 2, the preparation method of 2 '-dinitrobenzene dibenzyl, is characterized in that:
Sodium methylate is distributed in solvent paraffin oil, controls certain temperature of reaction, instills Ortho Nitro Toluene with methane amide simultaneously, then through insulation, hydrolysis, dealcoholysis, separation, washing, drying process obtained 2,2 '-dinitrobenzene dibenzyl finished product.
2. as claimed in claim 12, the preparation method of 2 '-dinitrobenzene dibenzyl, is characterized in that the mass ratio of sodium methylate and paraffin oil is 1:3.7 ~ 7.4.
3. one 2 as claimed in claim 1, the preparation method of 2 '-dinitrobenzene dibenzyl, is characterized in that: temperature of reaction is 5 ~ 10 DEG C.
4. one 2 as claimed in claim 1, the preparation method of 2 '-dinitrobenzene dibenzyl, is characterized in that: sodium methylate: Ortho Nitro Toluene: methane amide mol ratio is 1:1.95:2.
5. one 2 as claimed in claim 1, the preparation method of 2 '-dinitrobenzene dibenzyl, is characterized in that: Ortho Nitro Toluene is 5 ~ 10 DEG C with the dropping temperature of methane amide, and time for adding is 2.0 ~ 3.0 hours.
6. one 2 as claimed in claim 1, the preparation method of 2 '-dinitrobenzene dibenzyl, is characterized in that: insulation divides two sections and carries out, first paragraph 5 ~ 10 DEG C insulation 4 hours, second segment 10 ~ 15 DEG C insulation 6 hours.
7. one 2 as claimed in claim 1, the preparation method of 2 '-dinitrobenzene dibenzyl, is characterized in that: hydrolysis adds the heavy water of paraffin wet goods, and hydrolysis temperature is at 30 ~ 40 DEG C, and hydrolysis time 0.5 ~ 1 hour, hydrolysis water is the wash water jacket of upper batch.
8. one 2 as claimed in claim 1, the preparation method of 2 '-dinitrobenzene dibenzyl, is characterized in that: dealcoholysis is steamed except by-product methyl alcohol under referring to hydrolysate normal pressure or reduced pressure, and distillation temperature is no more than 95 DEG C.
9. one 2 as claimed in claim 1, the preparation method of 2 '-dinitrobenzene dibenzyl, is characterized in that: sepn process refers under 30 ~ 40 DEG C of conditions, press filtration or suction filtration are separated 2,2 '-dinitrobenzene dibenzyl crude product is with mother liquor, and the buck in mother liquor, can sell and produce for water reducer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410594600.5A CN104610065B (en) | 2014-10-22 | 2014-10-22 | A kind of 2, the preparation method of 2 '-dinitrobenzene dibenzyl |
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| CN201410594600.5A CN104610065B (en) | 2014-10-22 | 2014-10-22 | A kind of 2, the preparation method of 2 '-dinitrobenzene dibenzyl |
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| CN104610065A CN104610065A (en) | 2015-05-13 |
| CN104610065B true CN104610065B (en) | 2015-12-30 |
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| CN106749346A (en) * | 2016-12-21 | 2017-05-31 | 安徽金鼎医药股份有限公司 | A kind of new method for preparing adjacent dinitro dibenzyl |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1616433A (en) * | 2004-09-20 | 2005-05-18 | 俞锋 | Carbamazepine medicine and its preparing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1616433A (en) * | 2004-09-20 | 2005-05-18 | 俞锋 | Carbamazepine medicine and its preparing method |
Non-Patent Citations (1)
| Title |
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| 10，11-二氢-5H-二苯并[b，f]氮杂 合成方法的改进;汪海波;《中国医药工业杂志》;20011231;第32卷(第1期);第35-36页 * |
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Effective date of registration: 20200331 Address after: 016041 Lianxin Road, industrial park, Wuda District, Wuhai City, Inner Mongolia Autonomous Region (east side of Yiyang company) Patentee after: INNER MONGOLIA YUANHONG FINE CHEMICAL Co.,Ltd. Address before: 224555 Jiangsu province Yancheng City Binhai Industrial Zone head Zeng Patentee before: BINHAI BODA CHEMICAL Co.,Ltd. |
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