C07B33/00

Electrochemical deblocking solution for electrochemical oligomer synthesis on an electrode array
10006131 · 2018-06-26 · ·

There is disclosed an electrochemical deblocking solution for use on an electrode microarray. There is further disclosed a method for electrochemical synthesis on an electrode array using the electrochemical deblocking solution. The solution and method are for removing acid-labile protecting groups for synthesis of oligonucleotides, peptides, small molecules, or polymers on a microarray of electrodes while substantially improving isolation of deblocking to active electrodes. The method comprises applying a voltage or a current to at least one electrode of an array of electrodes. The array of electrodes is covered by the electrochemical deblocking solution.

METHODS OF PREPARING OXA-BICYCLOALKENE

Disclosed is a method of preparing an oxa-bicycloalkene via the reaction of a cycloalkanone and an allyl alcohol compound in the presence of an organic acid, a manganese catalyst, and oxygen at a predetermined temperature.

METHODS OF PREPARING OXA-BICYCLOALKENE

Disclosed is a method of preparing an oxa-bicycloalkene via the reaction of a cycloalkanone and an allyl alcohol compound in the presence of an organic acid, a manganese catalyst, and oxygen at a predetermined temperature.

PROCESS FOR THE PREPARATION OF A PURIFIED ACID COMPOSITION

A purified acid composition including 2,5-furandicarboxylic acid is prepared in a process, including oxidizing a feedstock containing 5-alkoxymethylfurfural to an oxidation product including 2,5-furandicarboxylic acid (FDCA) and 2-formyl-furan-5-carboxylic acid (FFCA), and esters of FDCA and, optionally, esters of FFCA; hydrolyzing the at least part of the oxidation product in the presence of water, thereby hydrolyzing at least esters of FDCA and, optionally, esters of FFCA to obtain an aqueous solution of an acid composition including FDCA, FFCA and ester of FDCA in an amount below the amount of ester of FDCA in the solution of the oxidation product; contacting at least part of the solution of the acid composition with hydrogen in the presence of a hydrogenation catalyst to hydrogenate FFCA to hydrogenation products, yielding a hydrogenated solution; and separating at least a portion of the FDCA from at least part of the hydrogenated solution by crystallization.

PROCESS FOR THE PREPARATION OF A PURIFIED ACID COMPOSITION

A purified acid composition including 2,5-furandicarboxylic acid is prepared in a process, including oxidizing a feedstock containing 5-alkoxymethylfurfural to an oxidation product including 2,5-furandicarboxylic acid (FDCA) and 2-formyl-furan-5-carboxylic acid (FFCA), and esters of FDCA and, optionally, esters of FFCA; hydrolyzing the at least part of the oxidation product in the presence of water, thereby hydrolyzing at least esters of FDCA and, optionally, esters of FFCA to obtain an aqueous solution of an acid composition including FDCA, FFCA and ester of FDCA in an amount below the amount of ester of FDCA in the solution of the oxidation product; contacting at least part of the solution of the acid composition with hydrogen in the presence of a hydrogenation catalyst to hydrogenate FFCA to hydrogenation products, yielding a hydrogenated solution; and separating at least a portion of the FDCA from at least part of the hydrogenated solution by crystallization.

PROCESS FOR THE PREPARATION OF A PURIFIED ACID COMPOSITION

A purified acid composition including 2,5-furandicarboxylic acid is prepared by a process including a) providing an acid composition solution of a crude acid composition in a polar solvent, the crude acid composition including 2,5-furandicarboxylic acid (FDCA) and 2-formyl-furan-5-carboxylic acid (FFCA); b) contacting the acid composition solution with hydrogen in the presence of a hydrogenation catalyst to hydrogenate FFCA to hydrogenation products, such that the hydrogenation products contain a minor amount of 2-methyl-furan-5-carboxylic acid (MFA) or no MFA, yielding a hydrogenated solution; c) separating at least a portion of the FDCA from the hydrogenated solution by crystallization.

PROCESS FOR THE PREPARATION OF A PURIFIED ACID COMPOSITION

A purified acid composition including 2,5-furandicarboxylic acid is prepared by a process including a) providing an acid composition solution of a crude acid composition in a polar solvent, the crude acid composition including 2,5-furandicarboxylic acid (FDCA) and 2-formyl-furan-5-carboxylic acid (FFCA); b) contacting the acid composition solution with hydrogen in the presence of a hydrogenation catalyst to hydrogenate FFCA to hydrogenation products, such that the hydrogenation products contain a minor amount of 2-methyl-furan-5-carboxylic acid (MFA) or no MFA, yielding a hydrogenated solution; c) separating at least a portion of the FDCA from the hydrogenated solution by crystallization.

PROCESS FOR THE SYNTHESIS OF IVACAFTOR AND RELATED COMPOUNDS

The present patent discloses a novel one pot two-step process for the synthesis of ivacaftor and related compounds of [Formula (I)], wherein R.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5, R.sup.6, R.sup.7 and Ar.sub.1 are as described above; its tautomers or pharmaceutically acceptable salts thereof starting from indole acetic acid amides.

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PROCESS FOR THE SYNTHESIS OF IVACAFTOR AND RELATED COMPOUNDS

The present patent discloses a novel one pot two-step process for the synthesis of ivacaftor and related compounds of [Formula (I)], wherein R.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5, R.sup.6, R.sup.7 and Ar.sub.1 are as described above; its tautomers or pharmaceutically acceptable salts thereof starting from indole acetic acid amides.

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Conversion of alcohols to carboxylic acids using heterogeneous palladium-based catalysts

Disclosed are methods for synthesizing an ester or a carboxylic acid from an organic alcohol. To form the ester one reacts, in the presence of oxygen gas, the alcohol with methanol or ethanol. This reaction occurs in the presence of a catalyst comprising palladium and a co-catalyst comprising bismuth, tellurium, lead, cerium, titanium, zinc and/or niobium (most preferably at least bismuth and tellurium). Alternatively that catalyst can be used to generate an acid from that alcohol, when water is also added to the reaction mix.