base protection oligonucleotide
A technology of oligonucleotides and bases, applied in the field of preparation of oligonucleotides, can solve the problems of determining the progress of the reaction, using excessive reagents and starting materials, and complexity
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[0208] In another embodiment, the present invention relates to a method for preparing an oligonucleotide, which comprises protecting the oligonucleotide with a base portion, wherein the nucleic acid base is protected with a C 5-30 straight chain or branched chain alkyl and / or C 5-30 The group protection of linear or branched alkenyl, the method preferably comprises the following steps (2):
[0209] (2) Make p-mer base protection oligonucleotide (p is any integer of 1 or greater) and n-mer oligonucleotide (n is an integer of 1 or greater) via its 5' hydroxyl The step of obtaining an n+p polymer oligonucleotide by condensation through a phosphite triester bond, in which the 3'-position hydroxyl group is phosphoramidated, and the 5'-position The hydroxyl group is protected by a temporary protecting group that can be removed under acidic conditions, and the nucleic acid base is protected by a C 5-30 straight chain or branched chain alkyl and / or C 5-30 The group protection of li...
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[0790] Hereinafter, the present invention is explained in more detail by referring to Preparations and Examples, which should not be construed as limiting the scope of the present invention. Reagents, equipment and materials used in the present invention are commercially available unless otherwise indicated. In this specification, when represented by an abbreviation, each represents a conventional abbreviation based on IUPAC-IUB Commission on Biochemical Nomenclature or the field.
[0791] The yields in the following Preparations and Examples represent mol / mol%. "%" in this specification means "% by mass" unless otherwise specified. In addition, the ratios of solvents in the following Preparations and Examples represent volume ratios. for 1 H-NMR spectrum, using tetramethylsilane as internal standard, using CDCl 3 Used as a measuring solvent. NMR spectra were measured using Bruker AVANCE AV300 (300MHz) nuclear magnetic resonance equipment or Bruker AVANCE 400 (400MHz) nuc...
preparation example 1
[0824] Preparation Example 1: Synthesis of 2,3-dihydrophytol
[0825] Phytol (10.00 g, 33.7 mmol) was dissolved in methanol, Pt / C (2%, 1.00 g) was suspended therein, and the suspension was stirred overnight under hydrogen atmosphere. After the reaction, the suspension was filtered to remove Pt / C, and the filtrate was concentrated to obtain 2,3-dihydrophytol. It was used in the next reaction without purification.
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