WO2018118525A1

WO2018118525A1 - Multi-well reaction block and method of assembly

Info

Publication number: WO2018118525A1
Application number: PCT/US2017/065784
Authority: WO
Inventors: Sarah TRICE
Original assignee: Sigma-Aldrich Co. Llc
Priority date: 2016-12-22
Filing date: 2017-12-12
Publication date: 2018-06-28

Abstract

A reaction block, comprising a base; a plurality of wells in the base, one or more of the wells holding a vial; a lid having a top surface and a bottom surface; and a single fastener and a spacer unit, the spacer unit being positioned on the top surface of the lid and secured to the lid by the fastener with sufficient force so as to seal the bottom surface of the lid to each of the vials.

Description

MULTI-WELL REACTION BLOCK AND METHOD OF ASSEMBLY CROSS-REFERENCE TO RELATED APPLICATIONS

[0001] This application claims the benefit of priority of

U.S. Provisional Patent Application No. 62/437,927 filed December 22, 2016, the entirety of which is hereby incorporated herein by reference.

BACKGROUND

[0002] Multi-well reaction blocks allow end-users to run multiple reactions in parallel, including reactions that are carried out at elevated temperatures, without solvent loss or solvent leaching. In addition, oxygen sensitive cross-coupling reactions can be run easily and robustly in a laboratory fume hood and under an inert atmosphere.

[0003] More specifically, conventional multi-well reaction blocks are designed to seal for minimal solvent loss. A torque screwdriver may be used to ensure sealing of the block to avoid over-tightening and stripping of sealing screws. The block must be sealed in a way that ensures that even pressure is applied; pressure application to the lid of the block must be applied evenly to keep the top cover flat while sealing.

[0004] To that end, multiple sealing screws are provided in the lid, strategically arranged. While pressure is applied to the center of the lid, a torque screwdriver is used to tighten each of the screws in a cross-pattern across the lid so that it is evenly sealed onto the base of the reaction block. In some cases, nine separate screws need to be individually manually tightened to properly and effectively secure the lid to the base of the reaction block. If the screws are not tightened in the correct order, the resulting seal may not be adequate to prevent solvent loss and contain energetic reactions. This process is time consuming and tedious, especially if done under a fume hood with gloves and safety googles on or in a glove box. [0005] It therefore would be desirable to provide a reaction block suitable for running multiple reactions in parallel that does not require the cumbersome and time consuming assembly of the conventional device.

SUMMARY

[0006] Problems of the prior art have been addressed by the embodiments disclosed herein, which relate to a reaction block having a single fastener and single spacer unit to seal the lid to the base. A single fastener and spacer unit allow for a simple and rapid assembly, and leads to less hand, wrist and lower arm stress experienced by users who prepare multiple blocks on a regular basis. In certain embodiments, the single fastener and spacer unit are configured such that is capable of applying sufficient pressure across the lid to effect a suitable seal to vials positioned in the base.

[0007] Accordingly, in some embodiments a reaction block is provided that comprising a base; a plurality of wells in the base, one or more of the wells holding a vial; a lid having a top surface and a bottom surface and a through aperture; and a single fastener and a single spacer unit, the spacer unit being positioned on the top surface of the lid and secured to the lid by the fastener with sufficient force so as to seal the bottom surface of the lid to each of the vials when the fastener is positioned in the through aperture and secured to the base.

BRIEF DESCRIPTION OF THE DRAWINGS

[0008] FIG. 1 is a cross-sectional view of a reaction block in accordance with certain embodiments;

[0009] FIG. 2 is a top perspective view of a reaction block base with the lid removed, in accordance with certain embodiments ;

[0010] FIG. 3 is a bottom perspective view of a reaction block base in accordance with certain embodiments; [0011] FIG. 4 is a top perspective view of a reaction block lid in accordance with certain embodiments;

[0012] FIG 5 is a bottom perspective view of a reaction block lid in accordance with certain embodiments;

[0013] FIG. 6A is a top view of a reaction block in accordance with an alternative embodiment; and

[0014] FIG. 6B is a cross-sectional view taken along line

6A-6A of FIG. 6A.

DETAILED DESCRIPTION

[0015] Although specific terms are used in the following description for the sake of clarity, these terms are intended to refer only to the particular structure of the embodiments selected for illustration in the drawings, and are not intended to define or limit the scope of the disclosure. In the drawings and the following description below, it is to be understood that like numeric designations refer to components of like function.

[0016] The singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise.

[0017] As used in the specification, various devices and parts may be described as "comprising" other components. The terms "comprise (s) ," "include (s) , " "having," "has," "can," "contain ( s ), " and variants thereof, as used herein, are intended to be open-ended transitional phrases, terms, or words that do not preclude the possibility of additional components.

[0018] All ranges disclosed herein are inclusive of the recited endpoint and independently combinable (for example, the range of "from 2 inches to 10 inches" is inclusive of the endpoints, 2 inches and 10 inches, and all the intermediate values .

[0019] As used herein, approximating language may be applied to modify any quantitative representation that may vary without resulting in a change in the basic function to which it is related. Accordingly, a value modified by a term or terms, such as "about" and "substantially," may not be limited to the precise value specified, in some cases. The modifier "about" should also be considered as disclosing the range defined by the absolute values of the two endpoints . For example, the expression "from about 2 to about 4" also discloses the range "from 2 to 4."

[0020] The terms "top" and "bottom" are relative to an absolute reference, i.e. the surface of the earth. Put another way, a top location is always located at a higher elevation than a bottom location, toward the surface of the earth.

[0021] Turning now to FIGS. 1-3, there is shown a reaction block 10 in accordance with certain embodiments. In some embodiments, the reaction block 10 includes a base 12 and a lid 14 configured to sealingly attach to the base 12. The base 12 and the lid 14 cooperate to form a block bounded by a bottom wall 15, side walls 16A, 16B, 16C and 16D and a top surface 17. A plurality of wells 18 (in certain embodiments, 24 such wells 18 are typical, although fewer or more could be used) are provided in the top surface 17 of base 12 and are each configured to receive a vial 20 or the like suitable for carrying out multiple reactions in parallel. In certain embodiments, each of the wells 18 is similarly dimensioned, but they need not be so. For example, FIGS. 6A and 6B illustrate a reaction block 10' that includes wells 118 of different dimensions (e.g., different diameters) . Thus, in the embodiment shown in FIG. 6A, there are two large wells 118A, and four medium wells 118B. In certain embodiments, the vials 20 are containers made of a suitable material that is not deleterious to the reaction taking place therein, such as glass; other suitable materials may include metal, such as stainless steel, or polymers suitable for the particular reactions. In some embodiments, the vials 20 are cylindrical tubes with a closed bottom and open top. Preferably each vial 20 and the respective well that it is positioned in are dimensioned so that the vial 20 is stable in the well and remains substantially vertically oriented therein. [0022] The reaction block 10, including base 12 and lid 14, is made of a material suitable to ensure adequate sealing for minimal solvent loss from vials 20. In some embodiments an external heat source may be used for heating the vials 20; in such embodiments, the reaction block 10 and in particular base 12 is made of a material suitable to allow transfer of heat from the external source to the vials 20. Further, in some embodiments, it may be desired to include magnetic stir bars in vials 20, making it desirable for reaction block 10 to be made of a non-magnetic material. In certain embodiments, base 12 and lid 14 are made of the same material, though in other embodiments, base 12 and lid 14 may be made of different materials. In a preferred embodiment, reaction block 10, including base 12 and lid 14 are made of anodized aluminum metal. Those skilled in the art can identify suitable materials that may be used.

[0023] In certain embodiments, each of the vials 20 has a length exceeding the depth of the well 18 (or 118) that it is received in, such that each vial 20 extends above the top surface 17 of the base 12, as seen in FIG. 2. In some embodiments, the depth of each well 18 (or 118) and the height of each vial 20 are such that all of the vials 20 extend from the top 17 of the base to the same extent. That is, the tops of the vials 20, when the vials 20 are positioned in the base 12, are substantially planar. In certain embodiments, each of the wells 18 are through- holes, with a bottom opening 21 having a diameter smaller than the outer diameter of the bottom of the vial 20, so that the vial 20 is supported therein. A gasket or O-ring 22 may be positioned in each well 18 near or at the bottom opening 21 to support the vial 20 (FIG. 3) . In other embodiments (FIG. 5B) , the each of the wells 118 may have a solid bottom.

[0024] FIGS. 4 and 5 illustrate a top or lid 14 for a reaction block in accordance with certain embodiments. In some embodiments, the lid 14 includes a plurality of apertures 25A- 25D each configured to receive a respective pin 26A-26D. Although four such apertures and four such pins 26A-26D are shown and preferred, fewer or more could be present. Each of the pins 26A- 26D may be made of steel or another suitable material, such as metals and metal alloys and composites, and extends through the lid 14 and is long enough to extend into corresponding apertures 36A-36D (FIG. 2) in the base 12 when the lid is aligned with and assembled to the base 12. In some embodiments, each of the pins is unthreaded. In certain embodiments, each pin 26A-26D may have a head that has a larger diameter than the pin body, and each aperture 25A-25D receiving a pin may be configured to have an annular seat on which the head of the pin sits to provide a stop so that the head of each pin is level or substantially level with the top surface 34 of the lid 14. In some embodiments, each of the pins 26A-26D is located at or near a corner of the lid 14.

[0025] In addition with assisting in aligning the lid 14 with the base 12 during assembly of the reaction block 10, the pins 26A-26D also aid in retaining one or more sealing members 30 such as gaskets that may be positioned between the bottom of the lid 14 and the vials 20 that are used to create a seal. In some embodiments, the sealing members 30 may be a silicone mat and a PFA (perfluoroalkoxy polymer resin) film, though other suitable materials for the sealing member may readily be determined by those skilled in the art. In some embodiments, two or more silicone mats may be used alone or together with a PFA film. Preferably the PFA film, when used, is the surface that contacts the vials 20.

[0026] In certain embodiments, the lid 14 has a generally centrally located through aperture 40 configured to receive fastener 44. Similarly, the base 12 has a generally centrally located aperture 41 that aligns with aperture 40 when the lid 14 is attached to the base 12. In some embodiments, at least a portion of the aperture 41 is internally threaded, and is dimensioned to receive fastener 44 that is itself externally threaded on at least a portion of its stem 45. In certain embodiments, threads 49 may be located at or near the bottom of the base 12 as shown in FIG. 1. In certain embodiments, threads 49 may be located at or near the top of the base as shown in FIG. 2. In some embodiments, the fastener 44 is may be made of steel and may be a #6 screw (thread diameter 0.138"; hole diameter 0.146") . Fasteners of other sizes and made of other metals may also be used.

[0027] In certain embodiments, a disk-shaped spacer unit 50, having a generally centrally located through aperture 51, distributes the load of the fastener over the lid 14 and provides suitable sealing pressure to seal the vials 20. The aperture 51 of spacer unit 50, may be threaded (e.g., a nut or threaded round spacer unit), partially threaded, or unthreaded (e.g., a washer, a stiffener, an unthreaded round spacer unit) . The aperture 51 is configured to receive the fastener 44, and may include an annular seat on which the head of the fastener sits to provide a stop and limit the extent to which the fastener 44 can penetrate into the aperture 51 of the spacer unit 50, into the aperture 40 of the lid 14, and into the aperture 41 of the base. In some embodiments, the bottom of the spacer unit 50 has an annular perimeter ring 52 that contacts the top surface 34 of the lid 14 when in the assembled condition. In certain embodiments, the spacer unit 50 may include an integral flange along its bottom edge. In certain embodiments, the spacer unit

50 is dimensioned such that it occupies a sufficient percentage of the top surface area of the lid 14 that when it is secured to the lid 14 (and thus the lid 14 to the base 12) by tightening of the fastener 44, an effective seal is created. For example, for a lid 14 that is about 2"(50.8 mm) L x 3" (76.2mm)W, a generally cylindrical spacer unit 50 having a diameter of about 1" (25.4mm) has been found to be suitable.

[0028] The spacer unit may be made of any suitable material, including, but not limited to metal and metal alloys, such as steel, aluminum, anodized aluminum, and so forth, or composite. While the spacer unit illustrated is shown as disk-shaped or approximately cylindrical, in other embodiments, the spacer unit may be square or rectangular as well. The single spacer unit described herein may be composed of more than one individual piece, e.g., a nut plus a washer or a nut plus a flattener, to form a single spacer unit of the desired dimensions. In still other embodiments, the fastener and spacer unit may be made as a single integral unit including the external threading elements of the fastener and the spacing and load distribution elements of the spacer unit, to ensure adequate sealing when the reaction block is fully assembled and sealed.

[0029] To assemble the reaction block 10, 10', the vials 20 are inserted into their respective wells 18, 118, and the lid 14 is positioned over the base 12, aligning each of the pins 26A-26D with its respective aperture 25A-25D in the base 12. The spacer unit 50 is then positioned on the top surface of the lid 14, and the fastener 44 is inserted into the aperture 51 of the spacer unit 50 and threadingly engaged with the threaded aperture 41 in base 12, such as with the aid of a torque screwdriver so as not to overtighten the fastener. It is noted that while preferred, the use of a torque screwdriver is not required. To further simplify assembly and disassembly of reaction block 10, 10', an electric screwdriver or electric torque screwdriver may be used. Those skilled in the art will appreciate that although a generally rectangular block is illustrated, other shapes, such as square or circular, can be used.

[0030] The term "consisting essentially of" is used herein to limit the scope of a claim to the specified materials or steps and those that do not materially affect the basic and novel characteristics of the claimed subject matter. The term permits the inclusion of elements which do not materially affect the basic and novel characteristics of the apparatus under conside ration , Accordi g1y, the expressions "consists essentially of" or "consisting essentially of" mean that the recited embodiment, feature, component, etc. must be present and that other embodiments, features, components, etc., may be present provided the presence thereof does not materially affect the performance, character or effect of the recited embodiment, feature, component, etc. For example, the use of more than one fastener would be considered to materially affect the basic and novel characteristics of the claimed subject matter. Similarly, additional method steps that add significant time to the assembly process would be considered to materially affect the basic and novel characteristics of the claimed subject matter.

Claims

What is claimed is:

1. A reaction block, comprising a base; a plurality of wells in the base, one or more of the wells holding a vial; a lid having a top surface and a bottom surface and an aperture through the top and bottom surfaces; and a single fastener and a single spacer unit, the spacer unit being positioned on the top surface of the lid and secured to the lid by the fastener with sufficient force so as to seal the bottom surface of the lid to each vial when the fastener is positioned in the aperture and attached to the base.

2. The reaction block of claim 1, further comprising a plurality of pins extending from the lid and into respective apertures of the base.

3. The reaction block of claim 2, wherein there are four pins.

4. The reaction block of claim 1, further comprising at least one sealing member positioned between the bottom surface of the lid and the top of each of the vials.

5. The reaction block of claim 4, wherein the at least one sealing member comprises a silicone mat.

6. The reaction block of claim 5, wherein the at least one sealing member further comprises a PFA film.

7. The reaction block of claim 1, wherein the base comprises 24 wells.

8. The reaction block of claim 1, wherein the base comprises wells of equal size.

9. The reaction block of claim 1, wherein the base comprises wells of different sizes.

10. The reaction block of claim 1, wherein the fastener is centrally located on the lid.

11. The reaction block of claim 1, further comprising an aperture in the base into which the fastener is attached.

12. The reaction block of claim 1, further comprising an aperture in the base into which the fastener is attached wherein the base aperture has a threaded portion that mates with a threaded portion of the fastener.

13. A reaction block, comprising a base; a plurality of wells in the base, one or more of the wells holding a vial, one or more alignment holes in the base, a central aperture in the base, the central aperture having a threaded portion therein; a lid having a top surface and a bottom surface, one or more alignment pins extending outwardly from the bottom surface and in alignment with the one or more alignment holes of the base and a central aperture in the lid and in alignment with the central aperture of the base; and a single spacer unit, the spacer unit being positioned on the top surface of the lid and secured to the lid by a fastener having a threaded portion on a lower portion for mating with the threaded portion of the aperture of the base with sufficient force so as to seal the bottom surface of the lid to each vial.

14. A reaction block, consisting essentially of a base; a plurality of wells in the base, one or more of the wells holding a vial; a lid having a top surface and a bottom surface; and a fastener and a spacer unit, the spacer unit being positioned on the top surface of the lid and secured to the lid by the fastener with sufficient force so as to seal the bottom surface of the lid to each vial.

A method of assembly a reaction block that comprises a base having a plurality of wells and a lid having a top surface and a bottom surface; the method comprising: introducing a vial into at least one of the plurality of wells in the base; aligning the lid with the base; providing a fastener and a spacer unit; securing the spacer unit to the top surface of the lid by attaching the lid to the base with the fastener with sufficient force so as to seal the bottom surface of the lid to the vial.