Apparatus and process for multiple chemical reactions

Chemical apparatus and process disinfecting – deodorizing – preser – Control element responsive to a sensed operating condition

Reexamination Certificate

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Details

C422S105000, C422S105000, C422S131000, C422S134000, C422S138000, C436S174000, C436S177000

Reexamination Certificate

active

06274091

ABSTRACT:

FIELD OF THE INVENTION
The invention relates to an apparatus and process for performing multiple chemical reactions, in particular for performing multiple solid phase chemical synthesis reactions and for isolating and collecting the final products of chemical reactions.
BACKGROUND OF THE INVENTION
One of the key processes in solid phase chemical synthesis is the washing of the solid support resin which has a chemical template attached thereto. Multiple washing cycles with different solvents ensures that all excess reagents used during reaction cycles are washed from the resin. A typical protocol involves addition of a wash solvent, shaking the resin with the solvent for five minutes and then removing the wash solvent from the reaction vessel. In many instances, the wash solvent is drained from the bottom of the reaction vessel by applying a vacuum, i.e., filtering the resin free of the waste solvent. The task is further complicated when multiple solid phase syntheses are simultaneously carried out.
For example, if each reaction vessel is to be subjected to a filtration step, performing separate filtration on each individual reaction vessel can be very time consuming. Alternatively, if filtering is to be performed on all of the reaction vessels simultaneously, this can lead to a very complicated and awkward arrangement of apparatus with, for example, each individual reaction vessel being connected to a vacuum source by a separate vacuum hose.
As described above, the waste liquid is flushed out during the washing cycles typically by vacuum filtration. During reaction cycles, however, the solvent and the reagents are to be retained in the reaction vessel which by design has a filter at the bottom. Previously, when batch filtering from several sources, each source was connected to the filter by a line with each line having a stop-cock or valve to regulate drainage.
SUMMARY OF THE INVENTION
An object of a first embodiment of this invention is to provide a reaction apparatus for performing multiple chemical reactions on solid support in a parallel fashion which provides stable support for multiple reaction vessels and permits such tasks as washing and filtering to be performed simultaneously on all the reaction vessels in a simple and easy manner through a manifold design. A further object is to provide an apparatus to be used in association with the reaction apparatus, for cleaving reaction products from the solid support and separately collecting the reaction products from each of the individual reaction vessels. Still a further object is to provide for the simultaneous release of fluid from reaction vessels.
Upon further study of the specification and appended claims, further objects and advantages of this invention will become apparent to those skilled in the art.
These objects are achieved at least in part in accordance with the invention by a reaction grid apparatus that can be used to perform multiple separate chemical reactions, the reaction grid comprising:
a first retaining member with a plurality of openings therethrough, each opening having an inlet and an outlet connected through a valve;
a separate reaction vessel for mounting in the inlet of each opening;
a drainage member having drainage channels therein aligned with the outlets of the bores; and
a valve operator for operating at least several of the valves simultaneously to drain fluids from the reaction vessels into the drainage member.
Also, in accordance with the invention, a cleavage block assembly is provided for separately collecting reaction products from multiple separate reactions, the cleavage block assembly comprising:
a vial rack capable of supporting an array of separate vials; a cleavage block section having a chamber therein for receiving the vial rack and a vacuum port for applying a vacuum to the chamber;
a reaction grid section having an array of openings therethrough, each opening corresponding in position to a position in the vial rack, the reaction grid section including a valve associated with each opening;
an array of reaction vessels mounted in the openings in the reaction grid and having reaction products therein; and
members for securing the reaction grid section to the cleavage block section in sealed relation therewith.
In accordance with the invention, the reaction reagents and solvents are contained within each of the reaction vessels.
Further, in accordance with a process aspect, the invention provides a process for performing multiple reactions and separately collecting reaction products, the process comprising:
connecting reaction vessels to valved openings through a manifold block of a reaction grid;
loading each of the reaction vessels with solid support beads and attaching chemical templates to the solid support beads via linkers;
performing chemical synthesis reactions for the preparation of organic molecules within each of the reaction vessels;
removing fluid from the reaction vessels by opening the valved openings to drain the fluid to a channeled block by applying a vacuum to the channeled block;
washing the solid support beads with wash solvent and removing the wash solvent from the reaction vessels by draining the wash solvent to a channel block;
removing the manifold block from connection with the channeled block and connecting the manifold block to a cleavage section, the cleavage section comprising a chamber containing a plurality of vial ports each holding a separate vial, each of the vial ports communicating with an inlet port of the manifold block, the cleavage section further comprising an outlet for connecting the chamber to a vacuum supply;
cleaving desired organic product from each of the reaction vessels and collecting the organic product within the individual vial.
The reaction grid in accordance with the invention enables the user to simultaneously carry out multiple chemical synthesis of desired molecules using solid phase chemical synthesis. Each of the multiple connection elements attached to the inlet ports of the reaction grid provide means for rigid and stable attachment of a reaction vessel such as a syringe barrel.
The reaction grid also allows the user to carry out several different steps in a chemical synthesis process in an integrated manner. Using standard protocols for solid phase synthesis, the reaction grid permits a user to simultaneously rinse or vacuum filter all of the reaction vessels. In addition, the user can perform different reactions simultaneously by utilizing different reagents in each of the reaction vessels during the synthesis mode. Furthermore, the reaction grid provides easy manipulation with respect to agitation. The reaction grid can be conveniently attached to a agitation device such as a wrist action shaker, vortexer or orbital shaker.
The plurality of inlet ports in the top surface of the reaction grid can be arranged in any suitable design. Preferably, the inlet ports are arranged in the form of a square or rectangular array having a certain number of rows and columns. A square or rectangular array is preferred for ease of formatting and tabulating individual chemical products obtained from a matrix synthesis.
The reaction grid can be designed to provide any desired number of inlet ports for attachment of reaction vessels. In a preferable arrangement, the reaction grid has
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inlet ports in a 12×8 array, this being the standard microtiter plate format used in industry for high throughput screening of compounds and biological assays. It is emphasized that other arrays, such as the smaller 5×8 array of parent application Ser. No. 08/532,279, filed Sep. 22, 1995, incorporated herein by reference, may be used in the practice of this invention.
Of course, even larger arrays, for example, a 100×100 matrix, can be provided in accordance with the invention. However, such large arrays require a large reaction grid which may require specialized agitation equipment and accessories for addition of solvents and reagents.
Each of the inlet ports is preferably equipped with a connection element that provides rigid and

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