Ethylene-glycol-alcoholized 3-pyridinol-4-ketone compound and preparation method and application thereof
A ketone compound, hydroxypyridine technology, applied in organic chemistry, drug combination, antidote, etc., can solve the problem of high drug price
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example 1
[0056] Example 1, the synthesis of 3-benzyloxy-2-methyl-4H-pyran-4-one
[0057]
[0058] Dissolve 122.3g NaOH in 278mL water, then add it into 1160mL ethanol solution containing 390g malt powder, mix well, add 422g benzyl chloride under stirring, heat and stir at 60°C for 3.5h after mixing well. After the reaction system is cooled, remove solid impurities by suction filtration, wash the filter residue with ethanol, spin dry after combining the washing liquid and the filtrate, dissolve the remaining substance with dichloromethane, then wash with 5wt% NaOH solution, and finally wash with water, and the organic layer After drying with anhydrous sodium sulfate and spin-drying the solvent, a light yellow oily liquid can be obtained. After cooling, recrystallize with ether to obtain the target product with a yield of 82%.
[0059] MS(ESI,m / z):[M+H] + calcd for C 13 h 13 o 3 217.09; found 217.10. 1 H NMR (CDCl 3 ):δ2.08(s,3H),5.16(s,2H),6.37(d,J=5.64Hz,1H),7.41-7.30(m,5H),7....
example 2
[0060] Example 2, the synthesis of 3-benzyloxy-2-ethyl-4H-pyran-4-one
[0061] Dissolve 122.3g NaOH in 278mL water, then add it into 1160mL ethanol solution containing 390g malt powder, mix well, add 422g benzyl chloride under stirring, heat and stir at 60°C for 3.5h after fully mixing; the reaction system is cooled Finally, remove solid impurities by suction filtration, wash the filter residue with ethanol, spin dry after combining the washing liquid and the filtrate, dissolve the remaining substance with dichloromethane, then wash with 5wt% NaOH solution, and finally wash with water, and wash the organic layer with anhydrous After drying with sodium sulfate, the solvent was spin-dried to obtain a light yellow oily liquid, which was recrystallized with ether after cooling to obtain the target product with a yield of 81%.
[0062]
example 3
[0063] Example 3, the synthesis of 3-benzyloxy-6-hydroxymethyl-4H-pyran-4-one
[0064]
[0065] Keeping the reaction conditions of Example 1 unchanged, malt powder was replaced by an equivalent amount of kojic acid to obtain 3-benzyloxy-6-hydroxymethyl-4H-pyran-4-one with a yield of 70%.
[0066] MS(ESI,m / z):[M+H] + calcd for C 13 h 13 o 4 233.08; found 233.17. 1 H NMR (DMSO-d 6 )δ: 4.30(s,2H), 4.95(s,2H), 5.71(br s,1H), 6.33(s,1H), 7.34-7.44(m,5H), 8.19(s,1H). 13 C NMR (DMSO-d 6 )δ: 173.17, 168.04, 146.58, 141.14, 136.12, 128.41(2C), 128.16, 128.11(2C), 111.12, 70.51, 59.28.
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