JP4583701B2 - Liquid phase automatic organic synthesizer - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention relates to an automatic synthesizing apparatus that performs supply of solvents and reagents, setting of reaction conditions, and separation and recovery of products in a liquid phase organic synthetic chemistry by computer control.
[0002]
[Prior art]
2. Description of the Related Art Conventionally, an automatic synthesizer that can efficiently add a reagent (raw material), react, separate, and recover by automatic control of a computer is known. (For example, patent document 1, patent document 2).
[0003]
An outline of the automatic synthesizing apparatus disclosed in Patent Documents 1 and 2 is shown in FIG. This automatic synthesizer comprises a reagent / solvent quantitative supply unit I, a reaction container unit II, an extraction / drying unit III, and a temperature control unit IV, and the reagent from the reagent / solvent quantitative supply unit I is reacted in the reaction container unit II. The product generated by the reaction is sent to the extraction / drying unit III, and the extracted / dried product is returned to the reaction vessel unit II again.
[0004]
[Patent Document 1]
JP-A-8-196897 [0030] to [0068], FIGS.
[Patent Document 2]
Japanese Patent Laid-Open No. 9-235241 [0023] to FIG.
[0005]
[Problems to be solved by the invention]
In the prior art described above, the reaction vessel constituting the reaction vessel unit II and other units are connected by individual tubes (piping). For example, the organic layer separated in the separation flask is guided to the drying tubes DT1 to DT1-3 of the extraction / drying unit III, dehydrated and dried, and then the reaction vessel of each reaction vessel unit II through the tubes t35, t36, and t37. To send it to.
For this reason, when the number of multistage reactions is increased or when the number of types of reactions is increased, the types of reagents and solvents required for the reaction increase, and as the number of reaction vessels increases, additional drying tubes and reaction vessels are added. Must. As described above, when the number of reaction systems in the conventional apparatus is increased, the number of units increases, and the number of pipes and changeover valves increases accordingly. This increases the size and complexity of the apparatus.
[0006]
[Means for Solving the Problems]
The purpose of this invention is to provide an automatic synthesizer that can increase or decrease the number of units by concentrating the piping and concentrating the piping in one place.
[0007]
That is, the automatic synthesizer according to the present invention includes a solvent unit including a plurality of containers for storing a solvent, for example, every predetermined amount, a reagent unit including a plurality of containers for storing a reagent, for example, every predetermined amount, A reaction unit that receives a solvent from a solvent unit and a reagent from a reagent unit and reacts a plurality of reagents, a separation unit that separates reaction products from the reaction unit, a recovery unit that collects reaction products, and a reaction product A drying unit for drying the product is provided, and the reaction product is transferred between the reaction unit, the liquid separation unit, the recovery unit, and the drying unit by a transfer unit.
By configuring in this way, there is no need to directly connect the reaction unit and the separation unit, the recovery unit or the drying unit by piping, and the open port of the multi-way valve in which the reaction container of the increased reaction unit is incorporated in the transfer unit It is enough to connect to
[0008]
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of the present invention will be described below with reference to the accompanying drawings. FIG. 1 is a front view of an automatic synthesizing apparatus according to the present invention, and FIG. 2 is a layout diagram of units constituting the automatic synthesizing apparatus.
[0009]
The automatic synthesizing apparatus divides an aluminum rack into a fixed area A and a variable area B. In the fixed area A, a cleaning unit 4, a liquid separation unit 5, a drying unit 6, a recovery unit 7 and a transfer unit 8 are arranged. .
The liquid separation unit 5 includes a centrifuge for eliminating the emulsion and a multi-way valve for switching the flow path to separate the reaction product from the reaction unit, and the drying unit 6 is a drying tube for drying the reaction product. The recovery unit 7 includes a plurality of containers for recovering the reaction product and a multi-way valve for switching the flow path.
[0010]
On the other hand, three sets of reagent units 10 and three sets of solvent units 11 are arranged in the upper stage of the variable region B where the number of units can be increased and decreased, and three sets of reaction units 12 are arranged in the middle stage.
[0011]
The computer 2 includes software for a synthesis apparatus control program for operating an electromagnetic valve, a relay, and the like, various unit operation programs for performing a reaction, and a synthesis procedure creation program for arranging the steps of the synthesis process. The experimenter selects a subroutine for the required operation and creates a synthesis program.
In executing the synthesis program, input conditions such as reaction temperature, reaction time, concentration temperature, concentration time, pH value, amount of solvent, addition of reagent, etc., and press the start button. As a result, the apparatus automatically starts the synthesis operation. In consideration of handling of substances harmful to the human body, remote control from another room is possible by connecting the computer 2 to a local area network and monitoring the apparatus with a camera.
[0012]
FIG. 3 is a piping diagram of the automatic synthesizer, FIG. 4 is a diagram illustrating the piping between the solvent unit, the reagent unit, and the reaction unit extracted from the piping of the automatic synthesizer, and FIG. 5 is the piping of the automatic synthesizer. It is the figure which extracted and showed the piping between a reaction unit, a liquid separation unit, a drying unit, and a collection | recovery unit. In the automatic synthesizer according to the present invention, the solvent, the reagent, the reactive organism, and the like are all transferred under reduced pressure, and therefore each unit is connected to a reduced pressure pump (VP.).
[0013]
The reagent unit 10 includes three reagent tubes 10a. The upstream portion of the reagent tube 10a is connected to a multi-way valve 10b, the first port of the multi-way valve 10b is connected to a decompression pump, the second port is connected to a nitrogen gas source, and the third port is connected to a reagent inlet. Is done.
The downstream part of the three reagent tubes 10a is connected to the first to third ports of the multi-way valve 10c, and the fourth port of the multi-way valve 10c is connected to another multi-way valve 10d.
Further, as described above, the first port of the multi-way valve 10d is connected to the fourth port of the multi-way valve 10c, the pipes t1 and t2 to the reaction unit are connected to the second port and the third port, and the fourth port is connected to the fourth port. Is connected to the pipe to the cleaning unit 4.
[0014]
The solvent unit 11 includes a multi-way valve 11a. A solvent bottle 11b (a commercially available solvent bottle can be used) is connected to the first port to the third port of the multi-way valve 11a, and a measuring tube 11c for measuring a fixed amount (20 ml) of solvent is connected to the fourth port. The pipes t3 and t4 to the reaction unit are connected to the fifth port and the sixth port, and the pipe to the cleaning unit 4 is connected to the seventh port.
[0015]
The reaction unit 12 is provided with a reaction vessel 13, a stirrer 14, a temperature adjustment bath 15, a filter 16 and a condenser 17, and further includes a multi-way valve for transferring with other units.
[0016]
That is, the pipes t1 and t2 from the reagent unit 10 are connected to the first port and the second port of the multi-way valve 12a, and the reaction vessel 13 is connected to the third port via the on / off valve.
In addition, pipes t3 and t4 from the solvent unit 11 are connected to the first port and the second port of the multi-way valve 12b, and the reaction vessel 13 is connected to the third port via an on / off valve.
A reactive organism take-out pipe t5 is connected to the first port of the multi-way valve 12c, a pipe t6 to the transfer unit 8 is connected to the second port, and a circulation pipe t7 to the filter 16 is connected to the third port. Is connected.
[0017]
The transfer unit 8 includes a multi-way valve 8a, a multi-way valve 8b, a multi-way valve 8c, and a multi-way valve 8d.
A pipe t6 from each reaction unit 12 is connected to the first port and the second port of the multi-way valve 8a , a pipe t8 from the liquid separation unit 5 is connected to the third port, and the multi-way valve is connected to the fourth port. 8b is connected.
Further, as described above, the multi-way valve 8a is connected to the first port of the multi-way valve 8b, the pipe t9 to the drying unit 6 is connected to the second port, and the multi-way valve 8c is connected to the third port. ing.
Further, the first port of the multiposition valve 8 c connected multiway valve 8b is as described above, the second port is connected to a pipe t10 from the drying unit 6, the multi-way valve 8d is connected to the third port Has been.
As described above, the multi-way valve 8c is connected to the first port of the multi-way valve 8d, the return pipe t11 to each reaction unit 12 is connected to the second port and the third port, and the fifth port is connected to the fifth port. A pipe t12 to the recovery unit 7 is connected, and a pipe t13 to the liquid separation unit 5 is connected to the sixth port.
[0018]
The liquid separation unit 5 is provided with a container 19 for receiving the organic phase and the aqueous phase separated from the centrifuge 18, and further includes a multi-way valve 5a and a multi-way valve 5b for transferring to another unit.
A pipe t13 from the transfer unit 8 is connected to the first port of the multi-way valve 5a, the second port is connected to the centrifuge 18, and the third port is connected to the container 19.
Further, the first port and the second port of the multi-way valve 5b are connected to each container 19, and a return pipe t8 to the transfer unit 8 is connected to the third port.
[0019]
The drying unit 6 is provided with a drying container 20 and further includes a multi-way valve 6a and a multi-way valve 6b.
A pipe t9 from the transfer unit 8 is connected to the first port of the multi-way valve 6a, and the drying container 20 is connected to the second to fourth ports.
The drying container 20 is connected to the first to third ports of the multi-way valve 6b, and the return pipe t10 to the transfer unit 8 is connected to the second port.
[0020]
A recovery flask 21 is attached to the recovery unit 7, and a multi-way valve 7 a that distributes a reaction product to each recovery flask 21 is provided.
[0021]
As described above, the reagent unit 10 and the solvent unit 11 and the reaction unit 12 are directly connected, but the reaction unit 12, the liquid separation unit 5, the drying unit 6 and the recovery unit 7 are connected via the transfer unit 8. Even if the number of reaction units 12 is increased, the configuration between the transfer unit 8, the liquid separation unit 5, the drying unit 6, and the recovery unit 7 does not change.
[0022]
【The invention's effect】
As described above, according to the automatic synthesizer according to the present invention, the transfer unit is provided in the apparatus, and the reaction unit and the separation unit, the recovery unit or the drying unit are connected via the transfer unit. Even if the number of units, solvent units and reaction units is increased, the number of pipes and valves between the transfer unit and the increased reaction unit will increase, but the pipe between the transfer unit and the separation unit, recovery unit or drying unit, etc. Therefore, the number of units can be increased or decreased, and the size and complexity of the automatic synthesizer can be avoided. In addition, in the case of a large apparatus, it is necessary to newly secure a place for installation. However, since the enlargement can be avoided, the apparatus can be stored in an existing draft or the like.
[Brief description of the drawings]
FIG. 1 is a front view of an automatic synthesizer according to the present invention. FIG. 2 is a layout diagram of units constituting the automatic synthesizer. FIG. 3 is a piping diagram of the automatic synthesizer. Fig. 5 shows the piping between the solvent unit, the reagent unit and the reaction unit extracted from the piping. Fig. 5 shows the piping between the reaction unit, the liquid separation unit, the recovery unit and the drying unit. Figure [Fig. 6] Piping diagram of conventional automatic synthesizer [Explanation of symbols]
A ... Fixed area, B ... Variable area, 1 ... Storage section for waste liquid tank, trap, pump, etc. 2 ... Control computer, 3 ... Relay and board storage section, 4 ... Cleaning unit, 5 ... Separation unit, 6 ... Drying unit, 7 ... Recovery unit, 8 ... Transfer unit, 8a ... Multi-way valve, 8b ... Multi-way valve, 8c ... Multi-way valve, 8d ... Multi-way valve, 10 ... Reagent unit, 10a ... Reagent tube, 10b ... Multi-way valve, 10c ... Multi-way valve, 10d ... Multi-way valve, 11 ... Solvent unit, 11a ... Multi-way valve, 11b ... Solvent bottle, 11c ... Measuring tube, 12 ... Reaction unit, 12a ... Multi-way valve, 12b ... Multi-way valve, 12c ... Multi-way valve , 13 ... Reaction vessel, 14 ... Stirrer, 15 ... Temperature control bath, 16 ... Filter, 17 ... Condenser, 18 ... Centrifuge, 19 ... Container, 20 ... Container for drying, 21 ... Recovery flask, t1- t13: piping.

Claims (2)

A plurality of containers for storing a solvent and a solvent unit having a multi-way valve for switching a flow path, a plurality of containers for storing a reagent and a reagent unit having a multi-way valve for switching a flow path, a multi-way valve for switching a flow path, and a temperature A reaction vessel for receiving a solvent from the solvent unit and a reagent from the reagent unit and reacting a plurality of reagents with a temperature control bath for adjusting the temperature, a temperature controller for adjusting the reaction temperature, and a stirrer, and a reaction having a condenser Separation unit for separating reaction product from reaction unit with multi-way valve for switching unit, centrifuge for eliminating emulsion and flow path, and multiple containers and flow paths for collecting reaction product Switch the recovery unit with a multi-way valve, and the drying pipe and flow path for drying the reaction product. In the automatic synthesizer provided with a drying unit having a way valve, the automatic synthesizer comprises a transfer unit for transferring reaction products between the reaction unit, the liquid separation unit, the recovery unit and the drying unit, and the transfer The unit is provided with four types of multi-way valves (8a, 8b, 8c, 8d). The multi-way valve (8a) is connected with a port to which piping from the reaction unit is connected and piping from the liquid separation unit. And a port connected to the multi-way valve (8b), the multi-way valve (8b) is connected to a port connected to the multi-way valve (8a), a port connected to the drying unit and a multi-way valve ( 8 c ), a port connected to the multi-way valve (8b), a port connected to the piping from the drying unit, and a multi-way valve (8d). The multi-way valve (8d) is connected to a port connected to the multi-way valve (8c), a port connected to the return pipe to the reaction unit, and a pipe to the recovery unit. And a port to which piping to the liquid separation unit is connected is provided.   2. The automatic organic synthesis apparatus according to claim 1, wherein the solvent unit, the reagent unit, and the reaction unit can be increased or decreased.

Images