CN211562128U

CN211562128U - Tazobactam intermediate synthesis impurity removal device

Info

Publication number: CN211562128U
Application number: CN201922334864.8U
Authority: CN
Inventors: 赵培新; 刘晓斐; 孙秀伟
Original assignee: Jinan Asia Pharma Tech Co ltd
Current assignee: Jinan Asia Pharma Tech Co ltd
Priority date: 2019-12-24
Filing date: 2019-12-24
Publication date: 2020-09-25
Anticipated expiration: 2029-12-24

Abstract

The utility model discloses a tazobactam intermediate synthesis impurity removal device, which comprises a filtering kettle body for receiving tazobactam intermediate synthesis liquid, a filter screen arranged at the inner side of the filtering kettle body, and diatomite arranged above the filter screen; an exhaust valve is arranged above the filter screen of the filter kettle body; the bottom of the filtering kettle body is connected to the layering kettle through a valve body; a stirrer is arranged in the layering kettle; a secondary extraction liquid inlet pipe is arranged on the layering kettle; the bottom of the layering kettle is connected with a U-shaped transparent pipe through a bottom valve; the U-shaped transparent pipe is connected to the distillation kettle through a flange; the bottom of the distillation kettle is connected to a tee joint through a valve body; a finished product valve is arranged at the bottom of the tee joint; the utility model discloses a synthetic edulcoration device of tazobactam midbody, synthetic feed liquid are in proper order through steps such as filtration, organic layer separation, organic layer extraction and solvent evaporation, and its edulcoration mode is simple and convenient, and the edulcoration is efficient.

Description

Tazobactam intermediate synthesis impurity removal device

Technical Field

The utility model particularly relates to a tazobactam midbody production facility, concretely relates to tazobactam midbody synthesis edulcoration device belongs to tazobactam midbody production facility technical field.

Background

Tazobactam is a novel blue enzyme alkyl sulfone beta-lactamase inhibitor after clavulanic acid and sulbactam, is an irreversible beta-lactamase inhibitor, has strong inactivation effect on A enzymes, has stronger enzyme inhibition effect than sulbactam, and has better stability than clavulanic acid; the antibacterial activity of the antibiotic can be enhanced, the antibacterial spectrum can be expanded, adverse reactions can be reduced, and the antibacterial peptide has a wide clinical application prospect; at present, the synthesis of tazobactam mainly comprises three synthesis routes according to different used starting materials, wherein (2S,5R) -3, 3-dimethyl-7-oxo-4-thia-1-azabicyclo [3.2.0] heptane-2-diphenylmethyl carboxylate 4-oxide is used as an intermediate to synthesize tazobactam most widely, while the impurity removal process in the production process of (2S,5R) -3, 3-dimethyl-7-oxo-4-thia-1-azabicyclo [3.2.0] heptane-2-diphenylmethyl carboxylate 4-oxide in the prior art is more complicated and has low impurity removal efficiency, so that the purification of products at the later stage is influenced.

SUMMERY OF THE UTILITY MODEL

In order to solve the problem, the utility model provides a synthetic edulcoration device of tazobactam midbody, its edulcoration mode is simple and convenient, and the edulcoration is efficient.

The utility model discloses a tazobactam midbody synthesizes edulcoration device, send into the filter kettle body through the synthetic feed liquid, carry out prefilter through the internal inboard diatomaceous earth of filter kettle, and send into the filtrating and separate into the layering cauldron, through standing separation for organic phase and aqueous phase, organic phase is separated the stills and is distilled, obtain the dope, the aqueous phase is squeezed into the dichloromethane through secondary extraction feed liquor pipe and is extracted, the extract is sent into the stills, and obtain mixed liquid after dissolving the dope in the stills, the mixed liquid is through the drying of drying cabinet back, send into the stills again through the backwash pump, the stills carry out the secondary evaporation, get rid of the dichloromethane in the mixed liquid, can obtain the product after the edulcoration, the product after the edulcoration is discharged from the finished product valve; the concrete structure is as follows: comprises a filtering kettle body for receiving tazobactam intermediate synthetic liquid, a filter screen arranged at the inner side of the filtering kettle body, and diatomite arranged above the filter screen; an external discharge valve is arranged above the filter screen of the filtering kettle body, and the external discharge valve can discharge diatomite periodically and feed new diatomite through the top of the filtering kettle body; the bottom of the filtering kettle body is connected to the layering kettle through a valve body; a stirrer is arranged at the inner side of the layering kettle; a secondary extraction liquid inlet pipe is arranged on the layering kettle; the bottom of the layering kettle is connected with a U-shaped transparent pipe through a bottom valve; the bottom of the U-shaped transparent pipe is provided with an emptying valve; the U-shaped transparent pipe is connected to the distillation kettle through a flange; the bottom of the distillation kettle is connected to a tee joint through a valve body; a finished product valve is arranged at the bottom of the tee joint; the middle end of the tee joint is connected to a drying tank through a drying valve; the other end of the drying tank is connected to the distillation kettle through a reflux pump.

In a preferred embodiment, a heating jacket is arranged outside the distillation kettle, and the heating jacket provides the primary evaporation heat and the secondary evaporation heat, so that the evaporation temperature can be adjusted.

As a preferred embodiment, the top of the drying tank is provided with a turnover cover; a filter screen framework is arranged in the middle of the inner side of the drying tank; a filter basket is arranged on the filter screen framework; the filter basket is provided with a drying filler, and the dehydration and drying tasks are completed through the drying filler; after the drying is finished, the anhydrous sodium sulfate can be filtered through the filter basket, and when the filter basket needs to be fed and taken out, the flip cover is directly opened.

As a preferred embodiment, the dry filler is anhydrous sodium sulfate.

In a preferred embodiment, the distillation still is provided with a solvent cooling recovery line, and the tetrahydrofuran-based organic solution is collected during the first evaporation and the dichloromethane solution is collected during the second evaporation.

Compared with the prior art, the utility model discloses a synthetic edulcoration device of tazobactam midbody, the feed liquid that the synthesis obtained is through steps such as filtration, organic layer separation, organic layer extraction and solvent evaporation in proper order, and its edulcoration mode is simple and convenient, and the edulcoration is efficient.

Drawings

Fig. 1 is a schematic view of the overall structure of embodiment 1 of the present invention.

Detailed Description

Example 1:

as shown in fig. 1, a tazobactam intermediate synthesis impurity removal device is characterized in that feed liquid obtained by synthesis is sent into a filter kettle body, preliminary filtration is carried out through diatomite on the inner side of the filter kettle body, filtrate is sent into a layering kettle, the filtrate is separated into an organic phase and a water phase through standing, the organic phase is separated into a distillation kettle and evaporated to obtain a sticky substance, the water phase is pumped into dichloromethane through a secondary extraction liquid inlet pipe for extraction, extract liquid is sent into the distillation kettle and dissolves the sticky substance in the distillation kettle to obtain a mixed liquid, the mixed liquid is dried through a drying tank and then is sent into the distillation kettle again through a reflux pump, the distillation kettle carries out secondary evaporation to remove dichloromethane in the mixed liquid, and a product after impurity removal can be obtained, and the product after impurity removal is discharged from a finished product valve; the concrete structure is as follows: comprises a filtering kettle body 1 for receiving tazobactam intermediate synthetic liquid, a filter screen 2 arranged on the inner side of the filtering kettle body, and diatomite 3 arranged above the filter screen; an external discharge valve 4 is arranged above the filter screen of the filtering kettle body 1, and the external discharge valve can discharge diatomite periodically and feed new diatomite through the top of the filtering kettle body; the bottom of the filtering kettle body 1 is connected to the layering kettle 5 through a valve body; a stirrer 6 is arranged at the inner side of the layering kettle 5; a secondary extraction liquid inlet pipe 7 is arranged on the layering kettle 5; the bottom of the layering kettle 5 is connected with a U-shaped transparent pipe 8 through a bottom valve; the bottom of the U-shaped transparent pipe 8 is provided with an emptying valve; the U-shaped transparent pipe 8 is connected to a distillation kettle 9 through a flange; the bottom of the distillation kettle 9 is connected to a tee joint 10 through a valve body; a finished product valve 11 is arranged at the bottom of the tee joint 10; the middle end of the tee joint 10 is connected to a drying tank 13 through a drying valve 12; the other end of the drying tank 13 is connected to the distillation still 9 through a reflux pump.

Wherein, a heating jacket 91 is arranged outside the distillation kettle 9, primary evaporation heat and secondary evaporation heat are provided by the heating jacket 91, and the evaporation temperature is adjustable; a flip cover 134 is arranged at the top of the drying tank 13, and a filter screen framework 131 is arranged in the middle of the inner side of the drying tank 13; a filter basket 132 is arranged on the filter screen framework 131; the filter basket 132 is provided with a dry filler 133, and the dehydration and drying tasks are completed through the dry filler; the dry filler 133 is anhydrous sodium sulfate, and after drying is completed, the anhydrous sodium sulfate can be filtered through the filter basket, and when the filter basket needs to be fed and taken out, the flip cover is directly opened.

In another embodiment, the distillation still 9 is provided with a solvent cooling recovery line 14 for collecting the tetrahydrofuran-based organic solution during the first evaporation and collecting the dichloromethane solution during the second evaporation.

The above-mentioned embodiment is only the preferred embodiment of the present invention, so all the equivalent changes or modifications made by the structure, features and principles of the present invention are included in the claims of the present invention.

Claims

1. A tazobactam intermediate synthesis impurity removing device is characterized in that: comprises a filtering kettle body for receiving tazobactam intermediate synthetic liquid, a filter screen arranged at the inner side of the filtering kettle body, and diatomite arranged above the filter screen; an exhaust valve is arranged above the filter screen of the filter kettle body; the bottom of the filtering kettle body is connected to the layering kettle through a valve body; a stirrer is arranged at the inner side of the layering kettle; a secondary extraction liquid inlet pipe is arranged on the layering kettle; the bottom of the layering kettle is connected with a U-shaped transparent pipe through a bottom valve; the bottom of the U-shaped transparent pipe is provided with an emptying valve; the U-shaped transparent pipe is connected to the distillation kettle through a flange; the bottom of the distillation kettle is connected to a tee joint through a valve body; a finished product valve is arranged at the bottom of the tee joint; the middle end of the tee joint is connected to a drying tank through a drying valve; the other end of the drying tank is connected to the distillation kettle through a reflux pump.

2. The tazobactam intermediate synthesis impurity removal device according to claim 1, wherein: and a heating jacket is arranged outside the distillation kettle.

3. The tazobactam intermediate synthesis impurity removal device according to claim 1, wherein: the top of the drying tank is provided with a turnover cover; a filter screen framework is arranged in the middle of the inner side of the drying tank; a filter basket is arranged on the filter screen framework; and the filter basket is provided with a dry filler.

4. The tazobactam intermediate synthesis and impurity removal device according to claim 3, wherein: the dry filler is anhydrous sodium sulfate.

5. The tazobactam intermediate synthesis impurity removal device according to claim 1, wherein: and a solvent cooling and recovering pipeline is arranged on the distillation kettle.