Novel siRNA chemical modification monomer, preparation method thereof and use thereof
A chemical modification and monomer technology, applied in chemical instruments and methods, organic chemistry, pharmaceutical formulations, etc., can solve problems such as poor biological stability, short half-life, and limited development
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Embodiment 1
[0037] "Example 1" Preparation of 2-hydroxyl-3-(4,4'-dimethoxytrityloxy) propyl phenyl ether
[0038] Take phenol (90mmol), 150mL of methyl ethyl ketone, and potassium carbonate (180mmol), add them into a 500mL three-necked reaction flask, and add epichlorohydrin (630mmol) dropwise under stirring at 45°C. After about 30 minutes, the dropwise addition is completed, and the reaction solution becomes cloudy , heated up to 80°C, refluxed for 10h, cooled, filtered, evaporated most of the solvent under reduced pressure, added 100mL of water, extracted with dichloromethane (100mL×3), washed the organic layer with 20% NaOH (10mL×3) times, organic The layer was dried over anhydrous magnesium sulfate, filtered, and dichloromethane was distilled off under reduced pressure. 2,3-Epoxypropylphenyl ether was obtained as a yellow oil.
[0039] Take the crude product of 2,3-epoxypropylphenyl ether (90mmol), water (90mmol), DMF (9mmol) into the reaction flask, seal it, heat up to 110°C and sti...
Embodiment 2
[0042] "Example 2" Preparation of 2-hydroxyl-3-(4,4'-dimethoxytrityloxy) propyl (4-fluoro)phenyl ether
[0043] 4-fluorophenol was used instead of phenol, and the operation method was referred to in Example 1 to obtain a light yellow oil with a yield of 71.0%.
[0044] 1H NMR (DMSO-d6, 400MHz) δ: 3.09 (d, J = 4.8Hz, 2H, CH2), 3.73 (s, 6H; 2OCH3), 4.04-4.13 (m, 3H; CH2CH), 5.29 (d, J = 4.8 Hz, 1H; OH), 6.89-6.97 (m, 6H; ArH), 7.08-7.54 (m, 11H; ArH).
Embodiment 3
[0045] "Example 3" Preparation of 2-hydroxyl-3-(4,4'-dimethoxytrityloxy) propyl (4-methyl)phenyl ether
[0046] 4-methylphenol was used instead of phenol, and the operation method was referred to in Example 1 to obtain a light yellow oil with a yield of 55.4%.
[0047] 1H NMR (DMSO-d6, 400MHz) δ: 2.21 (s, 3H; CH3), 3.07 (m, 2H; CH2), 3.72 (s, 6H; 2OCH3), 3.90-3.99 (m, 3H; CH2CH), 5.11 (d, J=4.8Hz, 1H; OH), 6.77(d, J=8.4Hz, 2H; ArH), 6.84-6.86(m, 4H; ArH), 7.05(d, J=8.4Hz, 2H; ArH ), 7.19-7.29 (m, 7H; ArH), 7.38 (d, J=7.6Hz, 2H; ArH).
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