CN109553571A - The method of chloro--methylpyridine is continuously prepared in a kind of microchannel - Google Patents
The method of chloro--methylpyridine is continuously prepared in a kind of microchannel Download PDFInfo
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- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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Abstract
The invention discloses a kind of methods that chloro--methylpyridine is continuously prepared in microchannel, which is characterized in that it includes the following steps: the preparation of step 1 benzyl propyl imines；The preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine；The preparation of step 3 chloro--methylpyridine.Using micro passage reaction as consersion unit, due to micro passage reaction large specific surface area, heat-transfer capability is strong, mixing uniformity is good, and reaction efficiency can be improved, greatly shorten the reaction time, greatly improve production efficiency；Enlarge-effect is not present in micro passage reaction, it can be directly used for being mass produced, and it can be accurately to control reaction condition, ensuring to react continuous, smoothly, accurately to carry out, and reduce the generation of side reaction, product yield can be improved to 90% or more, reduce consumption of raw materials, continuous dosing, and the material handled in microchannel is less, improves the safety of production.
Description
Technical field:
The present invention relates to a kind of preparation method of chloro--methylpyridine, in particular to continuously prepared in a kind of microchannel
The method of chloro--methylpyridine.
Background technique:
Chloro--methylpyridine (2-Chloro-5-methylpyridine) is that imidacloprid synthesis, Acetamiprid etc. are important
The intermediate of pesticide, production method is more, mainly has: using n- benzyl-n- propylene yl acetamide as raw material production, with 3- first
Yl pyridines-n- oxide is that raw material produces and makees intermediate production with organic salt, and above-mentioned three kinds of main methods predominantly mix
It being stirred to react, needs to use more set stirred tanks for reaction vessel, the reaction time is long, consumption of raw materials is big, equipment energy consumption is high, and
There is also safety problems for more set reaction kettle simultaneous reactions.Further, that there are product yields is low, side reaction is more, produces for these techniques
The problems such as low separation of product content is difficult.
Micro- Chemical Engineering Technology is a kind of realization chemical process green, safe and efficient important method, and micro passage reaction is made
Core equipment for micro- Chemical Engineering Technology has become one of research hotspot.Micro passage reaction utilizes precision processing technology manufacture
Microreactor of the characteristic size between 10 to 300 μm (or 1000 μm), has the advantage that 1, reaction condition can
Accurately to control, operability is good, it is ensured that reaction smoothly, continuously, accurately carries out；2, large specific surface area, mass-transfer efficiency is high,
Be conducive to improve the efficiency of hybrid reaction；3, continuous dosing, and the material handled in microchannel is less, and production peace can be improved
Quan Xing；4, without enlarge-effect, production scale amplification is unrestricted.Currently, micro passage reaction using more and more extensive, but
It is not used for the relevant report of chloro--methylpyridine production, continuously prepares the chloro- 5- methyl pyrrole of 2- in a kind of microchannel
The method of pyridine still belongs to blank.
Summary of the invention:
The purpose of the present invention is to provide in a kind of product yield height, the microchannel that the reaction time is short, production security is high
The method for continuously preparing chloro--methylpyridine.
The present invention is implemented by following technical solution: a kind of method that chloro--methylpyridine is continuously prepared in microchannel,
Include the following steps: the preparation of step 1 benzyl propyl imines；The system of step 2 n- benzyl-n- methoxyl group -2,3- allylamine
It is standby；The preparation of step 3 chloro--methylpyridine；Wherein:
The preparation of the step 1 benzyl propyl imines: propionic aldehyde and benzylamine are prepared into benzyl by micro passage reaction reaction
Base propyl imines；
The preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine: by the benzyl propyl imines, toluene three
Ethamine and acetylation reagent are reacted by micro passage reaction prepares n- benzyl-n- methoxyl group -2,3- allylamine；
The step 3 chloro--methylpyridine preparation: by n- benzyl-n- methoxyl group -2,3- allylamine, amide
Class reactant and the solid phosgene being dissolved in organic solvent react final by micro passage reaction and prepare the chloro- 5- methyl pyrrole of 2-
Pyridine.
Further, the preparation of the step 1 benzyl propyl imines, the step 2 n- benzyl-n- methoxyl group -2,3-
In the preparation of allylamine and step 3 chloro--methylpyridine preparation, micro passage reaction is stainless steel microchannel
Reactor, internal diameter is 100-1000 μm, length 1-3m.
Further, the preparation of the step 1 benzyl propyl imines: by the propionic aldehyde and the benzylamine in molar ratio 1:
(1.1-1.2) is delivered in micro passage reaction, and control reaction temperature is 0-25 DEG C, reaction time 5-30s, is made primary and is produced
Object, a product are separated, and benzyl propyl imines is obtained.
Further, the preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine: the benzyl propyl is sub-
Amine and toluene, triethylamine and acetylation reagent are 1:(3.2-3.5 in molar ratio): (1.0-1.2): the ratio of (1.0-1.2) is defeated
Send to micro passage reaction, control reaction temperature be 10-50 DEG C, reaction time 10-40s, obtain secondary product, it is described
Secondary product is handled through water-washing desalting, obtains desalination product, and the desalination product is handled through piptonychia benzene, finally obtains n- benzyl
Base-n- methoxyl group -2,3- allylamine.
Further, the acetylation reagent is acetic anhydride or chloroacetic chloride.
Further, the step 3 chloro--methylpyridine preparation: n- benzyl-n- methoxyl group -2,3- propylene
Amine, the solid phosgene and the amides reactant are according to molar ratio 1:(2-2.5): (1.0-1.2) is added to microchannel plate
Answer in device, control reaction temperature be 30-150 DEG C, reaction time 20-40s, obtain chloro--methylpyridine crude product.
Further, in the step 3 chloro--methylpyridine preparation, the organic solvent is toluene, chlorobenzene or two
Any one in chloroethanes；The mass concentration for being dissolved in the solid phosgene of the organic solvent is 20%-40%.
Further, in the step 3 chloro--methylpyridine preparation, the obtained 2- chloro-5-methypyridine is thick
Product successively washed, neutralized, is acidified, layered shaping, obtains purification chloro--methylpyridine.
Further, the amides reactant is n, n- dimethylformamide, n, n- diethylformamide or n, n- bis-
Any one of butyl formamide
Advantages of the present invention: 1, using micro passage reaction as consersion unit, due to micro passage reaction specific surface area
Greatly, heat-transfer capability is strong, mixing uniformity is good, and reaction efficiency can be improved, and greatly shortens the reaction time, the reaction time is by routine
Batch production at least needs 2 hours, foreshortens to 1 minute or so, greatly improves production efficiency；2, due to microchannel plate
Device is answered to can be directly used for being mass produced, and can accurately control reaction condition there is no enlarge-effect, it is ensured that reaction can be with
Continuously, it smoothly, accurately carries out, product yield is improved from the 80% of traditional handicraft to 90% or more, and product selectivity is from tradition
The 85% of technique can be improved to 92% or more, and side reaction is reduced, and reduce consumption of raw materials；3, this method is answered using microchannel plate
Device carries out, continuous dosing, and the material handled in microchannel is less, improves the safety of production.
Specific embodiment:
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described reality
Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without creative efforts, belongs to guarantor of the present invention
The range of shield.
Embodiment 1
The method of chloro--methylpyridine is continuously prepared in a kind of microchannel comprising following steps:
The preparation of step 1 benzyl propyl imines: the ratio that propionic aldehyde and benzylamine are 1:1.1 in molar ratio is delivered to length
For 1.5m, internal diameter be 500 μm stainless steel micro passage reaction reaction in, control reaction temperature be 0 DEG C, flow velocity 18m/
A product is made in min, reaction time 5s, and one time product is separated through solid, and obtaining solid is benzyl propyl imines；
The preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine: by benzyl propyl imines and toluene, triethylamine second
Acid anhydrides is the stainless steel micro passage reaction that the ratio of 1:3.2:1:1 is delivered to that length is 2m, internal diameter is 700 μm in molar ratio
Reaction, control reaction temperature is 10 DEG C, flow velocity 12m/min, reaction time 10s, obtains secondary product, secondary product warp
Water-washing desalting processing, obtains desalination product, desalination product is handled through piptonychia benzene, finally obtains n- benzyl-n- methoxyl group -2,3-
Allylamine；
Step 3 chloro--methylpyridine preparation: by n- benzyl-n- methoxyl group -2,3- allylamine, n, n- dimethyl methyl
It is 3m that amide (DMF) and the solid phosgene (BTC) being dissolved in toluene, which are transported to length, and internal diameter is that 700 μm of stainless steel is micro- logical
In road reactor, control reaction temperature be 30 DEG C, flow velocity 9m/min, reaction time 20s, obtain chloro--methylpyridine
Crude product, chloro--methylpyridine crude product successively washed, neutralized, is acidified, layered shaping, obtains the purification chloro- 5- of 2-
Picoline；Wherein, n- benzyl-n- methoxyl group -2,3- allylamine, solid phosgene (BTC), n, n- dimethylformamide (DMF)
Molar ratio be 1:2:1, mass concentration of the solid phosgene in toluene be 20%.
Embodiment 2
The method of chloro--methylpyridine is continuously prepared in a kind of microchannel comprising following steps:
The preparation of step 1 benzyl propyl imines: the ratio that propionic aldehyde and benzylamine are 1:1.1 in molar ratio is delivered to length
For 1.5m, internal diameter be 500 μm stainless steel micro passage reaction reaction in, control reaction temperature be 15 DEG C, flow velocity 11.3m/
A product is made in min, reaction time 8s, and one time product is separated through solid, and obtaining solid is benzyl propyl imines；
The preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine: by benzyl propyl imines and toluene, triethylamine second
Acid anhydrides is the stainless steel microchannel plate that the ratio of 1:3.3:1.1:1.1 is delivered to that length is 2m, internal diameter is 700 μm in molar ratio
Answer device to react, control reaction temperature be 25 DEG C, flow velocity 4.8m/min, reaction time 25s, obtain secondary product, secondary production
Object is handled through water-washing desalting, obtains desalination product, and desalination product is handled through piptonychia benzene, finally obtains n- benzyl-n- methoxyl group-
2,3- allylamines；
Step 3 chloro--methylpyridine preparation: by n- benzyl-n- methoxyl group -2,3- allylamine, n, n- dimethyl methyl
It is 3m that amide (DMF) and the solid phosgene (BTC) being dissolved in toluene, which are transported to length, and internal diameter is that 700 μm of stainless steel is micro- logical
In road reactor, control reaction temperature be 80 DEG C, flow velocity 6m/min, reaction time 30s, obtain chloro--methylpyridine
Crude product, chloro--methylpyridine crude product successively washed, neutralized, is acidified, layered shaping, obtains the purification chloro- 5- of 2-
Picoline；Wherein, n- benzyl-n- methoxyl group -2,3- allylamine, solid phosgene (BTC), n, n- dimethylformamide (DMF)
Molar ratio be 1:2.2:1.1, mass concentration of the solid phosgene in toluene be 25%.
Embodiment 3
The method of chloro--methylpyridine is continuously prepared in a kind of microchannel comprising following steps:
The preparation of step 1 benzyl propyl imines: the ratio that propionic aldehyde and benzylamine are 1:1.2 in molar ratio is delivered to length
For 1.5m, internal diameter be 500 μm stainless steel micro passage reaction reaction in, control reaction temperature be 20 DEG C, flow velocity 11.3m/
A product is made in min, reaction time 8s, and one time product is separated through solid, and obtaining solid is benzyl propyl imines；
The preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine: by benzyl propyl imines and toluene, triethylamine second
Acid anhydrides is the stainless steel microchannel plate that the ratio of 1:3.4:1.1:1.1 is delivered to that length is 2m, internal diameter is 700 μm in molar ratio
Answer device to react, control reaction temperature be 40 DEG C, flow velocity 4m/min, reaction time 30s, obtain secondary product, secondary product
It being handled through water-washing desalting, obtains desalination product, desalination product is handled through piptonychia benzene, methoxyl group -2 n- benzyl-n- are finally obtained,
3- allylamine；
Step 3 chloro--methylpyridine preparation: by n- benzyl-n- methoxyl group -2,3- allylamine, n, n- dimethyl methyl
It is 3m that amide (DMF) and the solid phosgene (BTC) being dissolved in toluene, which are transported to length, and internal diameter is that 700 μm of stainless steel is micro- logical
In road reactor, control reaction temperature be 120 DEG C, flow velocity 5.1m/min, reaction time 35s, obtain the chloro- 5- methyl of 2-
Pyridine crude product, chloro--methylpyridine crude product successively washed, neutralized, is acidified, layered shaping, obtains purification 2-
Chloro-5-methypyridine；Wherein, n- benzyl-n- methoxyl group -2,3- allylamine, solid phosgene (BTC), n, n- dimethylformamide
(DMF) molar ratio is 1:2.3:1.2, and mass concentration of the solid phosgene in toluene is 32%.
Embodiment 4
The method of chloro--methylpyridine is continuously prepared in a kind of microchannel comprising following steps:
The preparation of step 1 benzyl propyl imines: the ratio that propionic aldehyde and benzylamine are 1:1.2 in molar ratio is delivered to length
For 1.5m, internal diameter be 500 μm stainless steel micro passage reaction reaction in, control reaction temperature be 25 DEG C, flow velocity 9m/
A product is made in min, reaction time 10s, and one time product is separated through solid, and obtaining solid is benzyl propyl imines；
The preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine: by benzyl propyl imines and toluene, triethylamine second
Acid anhydrides is the stainless steel microchannel plate that the ratio of 1:3.5:1.2:1.2 is delivered to that length is 2m, internal diameter is 700 μm in molar ratio
Answer device to react, control reaction temperature be 50 DEG C, flow velocity 3m/min, reaction time 40s, obtain secondary product, secondary product
It being handled through water-washing desalting, obtains desalination product, desalination product is handled through piptonychia benzene, methoxyl group -2 n- benzyl-n- are finally obtained,
3- allylamine；
Step 3 chloro--methylpyridine preparation: by n- benzyl-n- methoxyl group -2,3- allylamine, n, n- dimethyl methyl
It is 3m that amide (DMF) and the solid phosgene (BTC) being dissolved in toluene, which are transported to length, and internal diameter is that 700 μm of stainless steel is micro- logical
In road reactor, control reaction temperature be 150 DEG C, flow velocity 4.5m/min, reaction time 40s, obtain the chloro- 5- methyl of 2-
Pyridine crude product, chloro--methylpyridine crude product successively washed, neutralized, is acidified, layered shaping, obtains purification 2-
Chloro-5-methypyridine；Wherein, n- benzyl-n- methoxyl group -2,3- allylamine, solid phosgene (BTC), n, n- dimethylformamide
(DMF) molar ratio is 1:2.5:1.2, and mass concentration of the solid phosgene in toluene is 40%.
Embodiment 5
The present embodiment produces chloro--methylpyridine using laboratory method, and 1mol benzylamine is added to three-necked flask,
0.91mol propionic aldehyde is slowly dropped into three-necked flask with dropping funel, after maintaining the temperature at 10 DEG C, reaction 3 hours, by what is obtained
Reaction product is separated by seperator, is separated into water and benzyl propyl imines, detects benzyl third through gas chromatograph
The yield of base imines is 93.1%, and selectivity is 95.0%.Benzyl propyl imines, toluene, triethylamine are added according to molar ratio
Enter three-necked flask, acetic anhydride is slowly dropped into three-necked flask, benzyl propyl imines, toluene, triethylamine and acetic acid with dropping funel
Molar ratio be maintained at 1:3.5:1.1:1.1, keep temperature constant at 25 DEG C.After reaction 3 hours, the reaction product that will obtain
Water-washing desalting operation is carried out, and the reaction of piptonychia benzene is carried out to the product after desalination, obtains n- benzyl-n- methoxyl group -2,3- third
Enamine.Yield through gas chromatograph detection n- benzyl-n- methoxyl group -2,3- allylamine is 96.3%, is selectively
97.2%.By n- benzyl-n- methoxyl group -2,3- allylamine, n, three-necked flask is added in n diformazan, with dropping funel by solid phosgene
It is slowly dropped into three-necked flask, by n- benzyl-n- methoxyl group -2,3- allylamine, solid phosgene, n, mole of n dimethyl formyl
Than being maintained at 1:2.3:1.1, keep temperature constant at 30 DEG C.Reaction 4 hours after, obtained reaction product is washed, in
With acidification, layering, final rectifying obtains chloro--methylpyridine.Receipts through gas chromatograph detection chloro--methylpyridine
Rate is 85.1%, and selectivity is 88.2%.
Table 1 is embodiment 1-5, the yield and selectivity statistics of intermediate products and final products chloro--methylpyridine
Table, seen from table 1, this method prepare chloro--methylpyridine using microchannel method, not only intermediate obtained in each step to produce
The yield of object is higher, and the yield of final products chloro--methylpyridine is also higher, meanwhile, comparative example 5 and other
The yield of each intermediate products and final products in embodiment is it is found that this method prepares the chloro- 5- methyl pyrrole of 2- using microchannel method
The yield of pyridine, intermediate products and final products is above the yield of produced in conventional processes, it is seen that chloro- using this programme preparation 2-
Enlarge-effect is not present in 5- picoline；And the intermediate products of embodiment 1-5 and the selectivity of final products are higher, base
This is higher than the selectivity of each intermediate products of embodiment 5 and final products, it is seen that this method produces chloro--methylpyridine
Side reaction is less, is suitble to industry expanding production.
1 embodiment 1-5 of table produces intermediate products and final products yield and selective statistical form
| Parameter | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Benzyl propyl imines selectivity (%) | 97.6 | 98.0 | 99.2 | 98.3 | 95.0 |
| Benzyl propyl imines yield (%) | 97.2 | 97.3 | 98.5 | 98.0 | 93.1 |
| N- benzyl-n- methoxyl group -2,3- allylamine selectivity (%) | 98.1 | 98.4 | 99.0 | 98.6 | 97.2 |
| N- benzyl-n- methoxyl group -2,3- allylamine yield (%) | 97.9 | 98.1 | 98.5 | 98.2 | 96.3 |
| Chloro--methylpyridine selectivity (%) | 92.0 | 95.4 | 97.3 | 96.8 | 88.2 |
| Chloro--methylpyridine yield (%) | 90.4 | 93.6 | 96.0 | 95.3 | 85.1 |
Claims (9)
1. continuously preparing the method for chloro--methylpyridine in a kind of microchannel, which is characterized in that it includes the following steps: to walk
The preparation of rapid benzyl propyl imines；The preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine；The chloro- 5- first of step 3 2-
Yl pyridines preparation；Wherein:
The preparation of the step 1 benzyl propyl imines: propionic aldehyde and benzylamine are prepared into benzyl propyl by micro passage reaction reaction
Imines；
The preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine: by the benzyl propyl imines, toluene triethylamine
Preparation n- benzyl-n- methoxyl group -2,3- allylamine is reacted by micro passage reaction with acetylation reagent；
The step 3 chloro--methylpyridine preparation: n- benzyl-n- methoxyl group -2,3- allylamine, amides are reacted
Object and the solid phosgene being dissolved in organic solvent are reacted by micro passage reaction finally prepares chloro--methylpyridine.
2. the method for continuously preparing chloro--methylpyridine in a kind of microchannel according to claim 1, feature exist
In, the preparation of the step 1 benzyl propyl imines, the preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine with
And in the step 3 chloro--methylpyridine preparation, micro passage reaction is stainless steel micro passage reaction, and internal diameter is
100-1000 μm, length 1-3m.
3. the method for continuously preparing chloro--methylpyridine in a kind of microchannel according to claim 1 or claim 2, feature exist
In the preparation of the step 1 benzyl propyl imines: the propionic aldehyde and the benzylamine 1:(1.1-1.2 in molar ratio) is delivered to
In micro passage reaction, control reaction temperature be 0-25 DEG C, reaction time 5-30s, be made a product, a product
It is separated, obtains benzyl propyl imines.
4. the method for continuously preparing chloro--methylpyridine in a kind of microchannel according to claim 1 or claim 2, feature exist
In the preparation of step 2 n- benzyl-n- methoxyl group -2,3- allylamine: by the benzyl propyl imines and toluene, triethylamine
In molar ratio it is 1:(3.2-3.5 with acetylation reagent): (1.0-1.2): the ratio of (1.0-1.2) is delivered to micro passage reaction
It is interior, control reaction temperature be 10-50 DEG C, reaction time 10-40s, obtain secondary product, the secondary product is through water-washing desalting
Processing, obtains desalination product, the desalination product is handled through piptonychia benzene, finally obtains n- benzyl-n- methoxyl group -2,3- propylene
Amine.
5. the method for chloro--methylpyridine is continuously prepared in a kind of microchannel according to claim 4, which is characterized in that
The acetylation reagent is acetic anhydride or chloroacetic chloride.
6. the method for continuously preparing chloro--methylpyridine in a kind of microchannel according to claim 1 or claim 2, feature exist
In the step 3 chloro--methylpyridine preparation: n- benzyl-n- methoxyl group -2,3- allylamine, the solid phosgene
With the amides reactant according to molar ratio 1:(2-2.5): (1.0-1.2) is added in micro passage reaction, control reaction
Temperature is 30-150 DEG C, reaction time 20-40s, obtains chloro--methylpyridine crude product.
7. the method for continuously preparing chloro--methylpyridine in a kind of microchannel according to claim 1, feature exist
In in the step 3 chloro--methylpyridine preparation, the organic solvent is any in toluene, chlorobenzene or dichloroethanes
It is a kind of；The mass concentration for being dissolved in the solid phosgene of the organic solvent is 20%-40%.
8. the method for continuously preparing chloro--methylpyridine in a kind of microchannel according to claim 6, feature exist
In in the step 3 chloro--methylpyridine preparation, the obtained chloro--methylpyridine crude product successively carries out water
It washes, neutralize, being acidified, layered shaping, obtaining purification chloro--methylpyridine.
9. according to claim 1, which is characterized in that the amides reactant is n, n- dimethylformamide, n, n-
Diethylformamide or n, n- dibutyl formamide any one.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102285913A (en) * | 2010-06-18 | 2011-12-21 | 北京英力精化技术发展有限公司 | Synthesis method of CMP (2-chloro-5-methylpyridine) |
| CN105330592A (en) * | 2015-11-23 | 2016-02-17 | 上海晋景化学有限公司 | Preparation method of 2-chloro-5-picoline |
| CN106117128A (en) * | 2016-06-26 | 2016-11-16 | 江苏扬农化工集团有限公司 | A kind of micro passage reaction prepares the method for pyridone chlorine addition product continuously |
| CN106810492A (en) * | 2017-01-24 | 2017-06-09 | 江苏扬农化工集团有限公司 | A kind of continous way prepares the industrialized preparing process of the picoline of 2 chlorine 5 |
-
2018
- 2018-11-29 CN CN201811443784.XA patent/CN109553571A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102285913A (en) * | 2010-06-18 | 2011-12-21 | 北京英力精化技术发展有限公司 | Synthesis method of CMP (2-chloro-5-methylpyridine) |
| CN105330592A (en) * | 2015-11-23 | 2016-02-17 | 上海晋景化学有限公司 | Preparation method of 2-chloro-5-picoline |
| CN106117128A (en) * | 2016-06-26 | 2016-11-16 | 江苏扬农化工集团有限公司 | A kind of micro passage reaction prepares the method for pyridone chlorine addition product continuously |
| CN106810492A (en) * | 2017-01-24 | 2017-06-09 | 江苏扬农化工集团有限公司 | A kind of continous way prepares the industrialized preparing process of the picoline of 2 chlorine 5 |
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Application publication date: 20190402 |