# US 2016/0354751 A1 · Neutralization and Containment of Redox Species Produced by Circumferential Electrodes

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- Number: US 2016/0354751 A1
- Document ID: US20160354751A1
- Status: Published application
- Kind: A1
- Application number: 15/208,606
- Filed: 2016-07-13
- Published: 2016-12-08
- Earliest claimed: 2005-04-15
- Assignees: CustomArray, Inc.
- Applicants: Customarray, Inc.
- Inventors: Karl Maurer; John J Cooper, Jr.; H Sho Fujii; Joseph Leonetti
- Web page: https://patentgrep.com/patent/US20160354751A1

## CPC

- B01J 19/0046: {Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays (synthesis methods per se C40B50/00)}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C25B 3/29: Coupling reactions
- C25B 9/17: Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
- C25B 11/02: characterised by shape or form
- B01J 2219/00527: Sheets
- B01J 2219/00529: DNA chips
- B01J 2219/00576: fluorophore
- B01J 2219/00585: Parallel processes
- B01J 2219/00596: Solid-phase processes
- B01J 2219/00641: the porous medium being continuous, e.g. porous oxide substrates
- B01J 2219/00653: the compounds being bound to electrodes embedded in or on the solid supports
- B01J 2219/00659: Two-dimensional arrays
- B01J 2219/00675: In-situ synthesis on the substrate
- B01J 2219/00713: Electrochemical synthesis
- B01J 2219/00722: Nucleotides
- B01J 2219/00725: Peptides
- B01J 2219/00731: Saccharides
- B01J 2219/00736: Non-biologic macromolecules, e.g. polymeric compounds
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C25B: ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR (anodic or cathodic protection C23F13/00; single-crystal growth C30B)

## Abstract

There is disclosed an electrode array architecture employing continuous and discontinuous circumferential electrodes. There is further disclosed a process for the neutralization of acid generated at anode(s) by base generated at cathode(s) circumferentially located to each other so as to confine a region of pH change. The cathodes can be displayed as concentric rings (continuous) or as counter electrodes in a cross pattern (discontinuous). In this way reagents, such as acid, generated in a center electrode are countered (neutralized) by reagents, such as base, generated at the corners or at the outer ring.

## Claims

### Claim 1

A method for electrochemical oligomer synthesis on a dense electrode array when electrode margins are 50 microns or less distance from each other, comprising:
(a) providing a dense electrode array having separately addressable electrodes;
(b) contacting the dense electrode array with an electrochemical deblocking solution; and
(c) conducting a deblocking step by addressing each active electrode with a first current or a first voltage, where each active electrode is surrounded by at least two neighboring electrodes that are biased with a second current or a second voltage as counter electrodes.

### Claim 2 (depends on 1)

The method of claim 1, where the deblocking step addresses each active electrode with the first current.

### Claim 3 (depends on 1)

The method of claim 1, where the at least two neighboring electrodes include at least four neighboring electrodes.

### Claim 4 (depends on 1)

The method of claim 1, where the at least two neighboring electrodes are arranged in a pattern selected from the group consisting of nearest neighbor, neighbor electrodes, border of neighbor electrodes, border of nearest-neighbor, one closest available electrode, and electrode that is not approach.

### Claim 5 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 10% acetonitrile; and
an upper limit of approximately 99% acetonitrile.

### Claim 6 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 1% methanol; and
an upper limit of approximately 90% methanol.

### Claim 7 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 1% dichloromethane; and
an upper limit of approximately 99% dichloromethane.

### Claim 8 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 1% isopropanol; and
an upper limit of approximately 99% isopropanol.

### Claim 9 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 0.01 mM dimethyl pyridine; and
an upper limit of approximately 200 mM dimethyl pyridine.

### Claim 10 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 0.1 mM benzoquinone; and
an upper limit of approximately 100 mM benzoquinone.

### Claim 11 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 0.1 mM hydroquinone; and
an upper limit of approximately 100 mM hydroquinone.

### Claim 12 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 0.1 mM tetraethylammonium p-toluenesulfonate; and
an upper limit of approximately 5 M tetraethylammonium p-toluenesulfonate.

### Claim 13 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 0.01 mM of a lutidine derivative; and
an upper limit of approximately 200 mM of a lutidine derivative.

### Claim 14 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 0.1 mM of a hydroquinone derivative; and
an upper limit of approximately 100 mM of a hydroquinone derivative.

### Claim 15 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes between:
a lower limit of approximately 0.1 mM of a benzoquinone derivative; and
an upper limit of approximately 100 mM of a benzoquinone derivative.

### Claim 16 (depends on 1)

The method of claim 1, where the electrochemical deblocking solution includes tetraethylammonium p-toluenesulfonate and lutidine, where the tetraethylammonium p-toluenesulfonate is dissolved in a solvent to form a first solution and the lutidine provides basicity to quench acidity of the tetraethylammonium p-toluenesulfonate in the first solution.

### Claim 17

A method of electrochemical deblocking an oligomer comprising the steps of:
covering an array of electrodes with a deblocking solution including:
lutidine, benzoquinone, hydroquinone and tetraethylammonium p-toluenesulfonate; and
one or more solvents selected from the group consisting of an alcohol, acetonitrile and dichloromethane; and
applying one or both a voltage and a current to at least one electrode of the array of electrodes.

### Claim 18 (depends on 17)

The method of claim 17, where the one or more solvents is between:
a lower limit of approximately 10% acetonitrile; and
an upper limit of approximately 99% acetonitrile.

### Claim 19 (depends on 17)

The method of claim 17, where the one or more solvents is between:
a lower limit of approximately 1% methanol; and
an upper limit of approximately 90% methanol.

### Claim 20 (depends on 17)

The method of claim 17, where the one or more solvents is between:
a lower limit of approximately 1% dichloromethane; and
an upper limit of approximately 99% dichloromethane.

### Claim 21

A kit for electrochemical deblocking comprising:
an array of electrodes adapted to connect with one or both a voltage and a current source to apply one or both a voltage and a current to at least one electrode of the array of electrodes;
a deblocking solution including:
lutidine, benzoquinone, hydroquinone and tetraethylammonium p-toluenesulfonate; and
one or more solvents selected from the group consisting of an alcohol, acetonitrile and dichloromethane; and
instructions for one or both preparing the deblocking solution and applying one or both a voltage and a current to at least one electrode of the array of electrodes.