CN202400994U - Cyclization ester production device - Google Patents
Cyclization ester production device Download PDFInfo
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- CN202400994U CN202400994U CN2011205748078U CN201120574807U CN202400994U CN 202400994 U CN202400994 U CN 202400994U CN 2011205748078 U CN2011205748078 U CN 2011205748078U CN 201120574807 U CN201120574807 U CN 201120574807U CN 202400994 U CN202400994 U CN 202400994U
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Abstract
The utility model discloses a cyclization ester production device, which comprises a nitrosation reaction kettle, an alkylation reaction kettle, a distillation kettle, a cyclization reaction kettle and a crude product cyclization ester centrifugal machine which are serially connected and is characterized in that a chlorinated reaction kettle is serially connected between the alkylation reaction kettle and the distillation kettle, a solid-product outlet of the crude product cyclization ester centrifugal machine is communicated with a refining kettle, and the outlet of the refining kettle is communicated with a refined product cyclization ester centrifugal machine. The cyclization ester production device is low in production cost, high in product yield rate, safe in production process and capable of producing products with low chroma and high purity.
Description
Technical field
The utility model relates to pharmaceutical chemistry technical field, relates in particular to a kind of cyclized ester production unit.
Background technology
Cyclized ester; Claim the ainothiazoly loximate ethyl ester again; Chemistry 2-(thiazolamine-4-yl) by name-2-methoxyimino ETHYLE ACETATE; Be a kind of important medicine intermediate, the cyclized ester product is mainly used in produces the AE active ester, so be used for synthesizing new efficiently antibiotics-third generation cephalosporin be cephalosporin.Cyclized ester is an important side chain midbody of producing third generation cephalosporins medicine; Cephalosporin microbiotic; Like: has a broad antifungal spectrum such as CEFOTAXIME SODIUM STERILE, rocephin, cefepime, cefpirome, antimicrbial power is strong, spinoff is little, in clinical application, replaces traditional microbiotic penicillium mould day by day.
Clearly propose in China's medical sci-tech development programs in 2010, develop the injection third generation cephalosporin selectively, the oral third generation cephalosporin of focus development, greatly develop the 4th generation cynnematin.Thereby domestic cynnematin development rapidly, also driven the development of cephalosporin intermediate cyclized ester ethyl ester.At present, China is the major country of production of cyclized ester, and products export is to a plurality of countries and regions, the world; Because cefotaxime, rocephin, cefetamet etc. contain the cynnematin of cyclized ester structure, have excellent curative effect, existing market is very good; And the novel anti rhzomorph that contains the cyclized ester structure is still being developed continuously; Therefore cyclized ester is as a kind of Medicine midbody, and market potential is huge, has a extensive future.
At present, the cyclized ester working method mainly contains enzymolysis process, " one pot " synthesis method, one pot " the low suitability for industrialized production that is unfavorable for of synthesis method repetition rate; industry in the most frequently used working method still by methyl aceto acetate through nitrosification, methylate, halogenation, four steps of ring-closure reaction process, this method technical maturity, reaction conditions is gentle; raw material be easy to get and produce in the recyclable utilization of solvent for use; but operational path is a polystep reaction, traditional production equipment be placed in-line nitrosation reaction still, alkylation reaction still, bromination reaction still and ring-closure reaction still in proper order, bromination reaction still cost is higher, yield is lower; generally about 67.5%; and operate and have certain danger, the product colourity of producing is higher, production unit is demanded improvement urgently.
The utility model content
The utility model technical problem to be solved is: to the deficiency that prior art exists, provide that a kind of production cost is low, product yield is high and the equipment of the production cyclized ester of production process safety.
For solving the problems of the technologies described above, the technical scheme of the utility model is:
A kind of cyclized ester production unit; Comprise mutual placed in-line nitrosation reaction still, alkylation reaction still, still kettle, ring-closure reaction still and bullion cyclized ester whizzer; Be in series with the chlorination still between said alkylation reaction still and the still kettle; The solid phase outlet of said bullion cyclized ester whizzer is communicated with refining kettle, and the outlet of said refining kettle is communicated with elaboration cyclized ester whizzer.
As a kind of scheme, the outlet of the liquid phase of said bullion cyclized ester whizzer is communicated with accumulator tank, and the outlet of said accumulator tank is communicated with the recovery still.
As a kind of scheme, the solid phase outlet of said elaboration cyclized ester whizzer is in series with vacuum drying oven in proper order, waves granulator and wrapping machine.
As a kind of improvement, the outlet of the liquid phase of said elaboration cyclized ester whizzer is communicated with mother liquor tank.
As a kind of scheme, the material inlet of said nitrosation reaction still is provided with the material dropper, and the outer wall of said nitrosation reaction still is provided with chuck.
As a kind of scheme, be in series with nitrosification thing storage tank between nitrosation reaction still and the alkylation reaction still, be in series with hydrocarbonylation thing storage tank between said alkylation reaction still and the chlorination still.
Owing to adopted technique scheme, the beneficial effect of the utility model is:
1, is in series with the chlorination still between hydrocarbonylation thing storage tank of the utility model and the still kettle; Substituted bromination reaction still of the prior art with the chlorination still; Replaced the difficult bromination reaction that carries out with chlorination, reduced production cost and operation easier, behind the improvement production equipment; Make material cost be reduced to 50,000 yuan per ton, yield reaches 70.8%; And the solid phase of the bullion cyclized ester whizzer of the utility model outlet is communicated with refining kettle, to the cyclized ester bullion carry out further refining after, the impurity in the product is removed, and has improved product purity; The outlet of said refining kettle is communicated with elaboration cyclized ester whizzer, and the elaboration cyclized ester is separated from mother liquor, obtains the product that colourity is low, purity is high.
2, the liquid phase of the bullion cyclized ester whizzer of the utility model outlet is communicated with accumulator tank, and the outlet of said accumulator tank is communicated with the recovery still, and the centrifugal cyclization mother liquor that comes out can get into accumulator tank and get into and reclaim still and recycle; The outlet of said elaboration cyclized ester whizzer is communicated with mother liquor tank, after can getting into mother liquor tank and collect from the centrifugal mother liquor that comes out of elaboration cyclized ester whizzer, is back to use the recycling of alkylation reaction still.
3, the utility model is provided with the material dropper at the material inlet of nitrosation reaction still, and during nitrosation reaction, material can be added dropwise to reaction kettle, and mixing of materials is even, has improved reaction effect.
Description of drawings
Accompanying drawing is the structural representation of the utility model embodiment.
Among the figure: 1. nitrosation reaction still, 11. material droppers, 12. chucks, 13. nitrosification thing storage tank, 2. alkylation reaction stills; 21. hydrocarbonylation thing storage tank, 3. chlorination still, 31. still kettles, 4. ring-closure reaction still, 41. bullion cyclized ester whizzers; 42. accumulator tank, 43. reclaim stills, 5. refining kettle, 51. elaboration cyclized ester whizzers; 52. mother liquor tank, 6. vacuum drying oven 7. waves granulator, 8. wrapping machine.
Embodiment
Below in conjunction with accompanying drawing and embodiment, further set forth the utility model.Should be understood that these embodiment only to be used to the utility model is described and be not used in the restriction the utility model scope.Should be understood that in addition those skilled in the art can do various changes or modification to the utility model after the content of having read the utility model instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Shown in accompanying drawing; A kind of cyclized ester production unit; Comprise mutual placed in-line nitrosation reaction still 1, nitrosification thing storage tank 13, alkylation reaction still 2, hydrocarbonylation thing storage tank 21, chlorination still 3, still kettle 31, ring-closure reaction still 4, bullion cyclized ester whizzer 41, refining kettle 5, elaboration cyclized ester whizzer 51, vacuum drying oven 6, wave granulator 7 and wrapping machine 8; The liquid phase outlet of said bullion cyclized ester whizzer 41 is communicated with accumulator tank 42; The outlet of said accumulator tank 42 is communicated with reclaims still 43, and the liquid phase outlet of elaboration cyclized ester whizzer 51 is communicated with mother liquor tank 52; Nitrosation reaction still 1 inner chamber top is provided with material dropper 11; Ring-closure reaction still 4 inner chamber tops are provided with the material dropper; Said nitrosation reaction still 1 outer wall is provided with chuck 12, and alkylation reaction still 2, chlorination still 3, ring-closure reaction still 4, refining kettle 5 and recovery still 43 outer walls are equipped with chuck.
The principle of work of the utility model is:
Methyl aceto acetate and Sodium Nitrite generate the nitrosification thing at the nitrosation reaction still 1 inner nitrosation reaction that takes place of the utility model; Nitrosification thing and methyl-sulfate generate the hydrocarbonylation thing at the alkylation reaction still 2 inner alkylation reactions that take place of the utility model; Hydrocarbonylation thing and chlorine generate the chloro thing at the chlorination still 3 inner chlorinations that take place of the utility model, and chloro thing and thiocarbamide/sodium-acetate/sheet alkali generates cyclocomplex at the ring-closure reaction still 4 inner ring-closure reactions that take place of the utility model; Cyclocomplex through bullion cyclized ester whizzer 41 centrifugally get rid of worry, washing obtains the cyclized ester bullion; The cyclized ester bullion is made with extra care in refining kettle 5; Centrifugally get rid of worrys, wash and obtain the elaboration cyclized ester through elaboration cyclized ester whizzer 51 then; The elaboration cyclized ester waves granulator 7 and pulverizes through vacuum drying oven 6 dryings, by wrapping machine 8 packings.
Claims (6)
1. cyclized ester production unit; Comprise mutual placed in-line nitrosation reaction still, alkylation reaction still, still kettle, ring-closure reaction still and bullion cyclized ester whizzer; It is characterized in that: be in series with the chlorination still between said alkylation reaction still and the still kettle; The solid phase outlet of said bullion cyclized ester whizzer is communicated with refining kettle, and the outlet of said refining kettle is communicated with elaboration cyclized ester whizzer.
2. a kind of cyclized ester production unit as claimed in claim 1 is characterized in that: the liquid phase outlet of said bullion cyclized ester whizzer is communicated with accumulator tank, and the outlet of said accumulator tank is communicated with the recovery still.
3. a kind of cyclized ester production unit as claimed in claim 1 is characterized in that: the solid phase outlet of said elaboration cyclized ester whizzer is in series with vacuum drying oven in proper order, waves granulator and wrapping machine.
4. a kind of cyclized ester production unit as claimed in claim 3 is characterized in that: the liquid phase outlet of said elaboration cyclized ester whizzer is communicated with mother liquor tank.
5. a kind of cyclized ester production unit as claimed in claim 1, it is characterized in that: the material inlet of said nitrosation reaction still is provided with the material dropper, and the outer wall of said nitrosation reaction still is provided with chuck.
6. like described any cyclized ester production unit of claim 1 to 5, it is characterized in that: be in series with nitrosification thing storage tank between nitrosation reaction still and the alkylation reaction still, be in series with hydrocarbonylation thing storage tank between said alkylation reaction still and the chlorination still.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011205748078U CN202400994U (en) | 2011-12-31 | 2011-12-31 | Cyclization ester production device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011205748078U CN202400994U (en) | 2011-12-31 | 2011-12-31 | Cyclization ester production device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202400994U true CN202400994U (en) | 2012-08-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011205748078U Expired - Fee Related CN202400994U (en) | 2011-12-31 | 2011-12-31 | Cyclization ester production device |
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| Country | Link |
|---|---|
| CN (1) | CN202400994U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110777178A (en) * | 2019-12-02 | 2020-02-11 | 河北慧林生物科技有限公司 | Application of immobilized carboxyl ester hydrolase in synthesis of side chains of cloxacillin, dicloxacillin, flucloxacillin and oxacillin |
-
2011
- 2011-12-31 CN CN2011205748078U patent/CN202400994U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110777178A (en) * | 2019-12-02 | 2020-02-11 | 河北慧林生物科技有限公司 | Application of immobilized carboxyl ester hydrolase in synthesis of side chains of cloxacillin, dicloxacillin, flucloxacillin and oxacillin |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120829 Termination date: 20181231 |