US 2025/0051256 A1 · PRODUCTION METHOD FOR PURIFIED DICHLOROACETIC ACID

Abstract

The present invention provides a production method for purified dichloroacetic acid and an efficient production method for a nucleic acid molecule using the same. Specifically, the present invention provides a production method for purified dichloroacetic acid having a molar ratio of formaldehyde to dichloroacetic acid of 81×10−5 or less and a molar ratio of dichloroacetic anhydride to dichloroacetic acid of 20×10−5 or less, the method including: bringing dichloroacetic acid having both or one of formaldehyde content and dichloroacetic anhydride content exceeding the ratio(s), into contact with at least one compound having a boiling point lower than that of dichloroacetic acid selected from the group consisting of aliphatic alcohols, aliphatic amines, and water, and, in the coexistence of an aprotic inert solvent having a boiling point lower than that of dichloroacetic acid, distilling off a fraction containing the solvent from the resulting mixed liquid, and a production method for a nucleic acid molecule using the purified dichloroacetic acid as a deprotecting agent.

Claims29

Dependent claims

A method for producing purified dichloroacetic acid, comprising:

contacting dichloroacetic acid with at least one compound selected from the group consisting of an aliphatic alcohol, an aliphatic amine, and water to obtain a mixed liquid;
causing the mixed liquid to coexist with an aprotic inert solvent having a boiling point lower than a boiling point of dichloroacetic acid;
and
distilling off a fraction containing the comprising a solvent from the resulting mixed liquid to produce purified dichloroacetic acid having a molar ratio of formaldehyde to dichloroacetic acid of 81×10−5 or less and a molar ratio of dichloroacetic anhydride to dichloroacetic acid of 20×10−5 or less,
wherein the at least one compound has a boiling point lower than a boiling point of the dichloroacetic acid, and
the dichloroacetic acid being contacted with the at least one compound satisfies at least one of i) and ii):
i) a formaldehyde content in the dichloroacetic acid exceeds the molar ratio of formaldehyde to dichloroacetic acid, and
ii) a dichloroacetic anhydride content in the dichloroacetic acid exceeds the molar ratio of dichloroacetic anhydride to dichloroacetic acid.

5 more elements

A method for producing a deprotected nucleic acid molecule by an amidite method, the method comprising:

preparing purified dichloroacetic acid having a molar ratio of formaldehyde to dichloroacetic acid of 81×10−5 or less and a molar ratio of dichloroacetic anhydride to dichloroacetic acid of 20×10−5 or less;
and
reacting the purified dichloroacetic acid with a nucleic acid molecule, having a protecting group protecting a hydroxyl group at the 5′-terminal, to remove the protecting group and produce the deprotected nucleic acid molecule.

Dependencies are inferred from the claim text.

Production method for purified dichloroacetic acid

Life of this patent

Production method for purified dichloroacetic acid

Life of this patent

Abstract

Claims29