Nucleic acid complex
A complex, nucleic acid technology, applied in the direction of sugar derivatives, drug combinations, genetic material components, etc., can solve the problem of specifically inhibiting the expression of APCS that has not yet been reported.
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[0917] Hereinafter, the present invention will be specifically described using reference examples, working examples, and test examples. However, the present invention is not limited to these Examples and Test Examples. It should be noted that the proton NMR spectra ( 1 H NMR) is measured at 270 MHz, 300 MHz, or 400 MHz, and the exchanged protons may not be clearly observed depending on the compound and measurement conditions. In addition, as an expression of the multiplicity of a signal, a commonly used expression is used, and br means broad, and represents an apparently wide signal.
[0918] The following conditions were used for the UPLC analysis.
[0919] Mobile phase A: aqueous solution containing 0.1% formic acid, B: acetonitrile solution
[0920] Gradient: 10%-90% linear gradient of mobile phase B (3 minutes)
[0921] Column: ACQUITY UPLC BEH C18 (1.7 μm, inner diameter 2.1×50 mm) manufactured by Waters Corporation
[0922] Flow rate: 0.8mL / min
[0923] PDA detecti...
reference example 1
[0956] [chemical formula 123]
[0957]
[0958] Synthesis of compound RE1-2
[0959] Reference Example 1 Process 1
[0960] Compound RE1-1 (0.8755 g, 1.9567 mmol) synthesized by the method described in Journal of American Chemical Society, vol. 136, pp. 16958-16961, 2014 was dissolved in tetrahydrofuran (10 mL), Add 1,3-dicyclohexylcarbodiimide (DCC, 0.4247g, 2.0584mmol) and N-hydroxysuccinimide (0.2412g, 2.0958mmol) and stir overnight at room temperature. The solid precipitated from the reaction mixture was removed, and the solvent was distilled off under reduced pressure. The resulting mixture was dissolved in N,N'-dimethylformamide (DMF), 2-aminoethylmaleimide bromate (0.6479 g, 2.5491 mmol) and diisopropylethylamine were added (1.7mL, 9.7835mmol), then stirred overnight at room temperature. Under reduced pressure, the solvent in the reaction solution was distilled off, and it was eluted by reversed-phase column chromatography (water / methanol=80 / 20), thereby obtainin...
reference example 2
[0972] [chemical formula 124]
[0973]
[0974] Reference Example 2 Process 1
[0975] ((2R,3R)-1,3-Dihydroxybutan-2-yl)(9H-fluoren-9-yl)methyl carbamate (compound RE2-1, manufactured by Chem-Impex International, Inc., 1.50 g, 4.58mmol) was dissolved in pyridine (20mL), and 4,4'-dimethoxytrityl chloride (manufactured by Tokyo Chemical Industry Co., Ltd., 1.71g, 5.04mmol) was added under ice-cooling, followed by stirring at room temperature 2 hours. The reaction solution was ice-cooled, 10% citric acid aqueous solution was added, extracted with ethyl acetate, the organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (hexane / ethyl acetate=90 / 10) to obtain compound RE2-2 (1.07 g, yield 37%).
[0976] ESI-MS m / z:630(M+H) +
[0977] Reference Example 2 Process 2
[0978]The compound RE2-2 (1.07g, 1.699mmol) synthesized ...
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