5-IODO-2-FUROIC ACID,97% synthesis
- Product Name:5-IODO-2-FUROIC ACID,97%
- CAS Number:18614-11-4
- Molecular formula:C5H3IO3
- Molecular Weight:237.98
88-14-2
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18614-11-4
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Yield:18614-11-4 88.1%
Reaction Conditions:
with sulfuric acid;dihydrogen peroxide in ethanol;lithium hydroxide monohydrate at 70; for 6 h;Cooling with ice;Reagent/catalyst;
Steps:
4; 1 Example 4
Iodination reaction: under stirring conditions, slowly add 2.5 g of concentrated sulfuric acid in 40 ml of solvent (ethanol: water = 1:3, v: v), then add 2.8 g (25 mmol) furan-2-carboxylic acid and 24.9 g (containing 25 mmol KI) KI/MC catalyst, and slowly add 30%H2O2dropwise under ice water bath conditions Solution 5.2 ml (50 mmol). After the dropwise addition, the temperature was increased to 70 °C for 6h, the thin layer chromatography (TLC) tracked the reaction, the raw material point disappeared, cooled to room temperature, and 0.1mol/L sodium bisulfite solution was added to decolorize until the color no longer changed. It was then extracted with dichloromethane, the organic phase was washed with saturated NaHCO3 solution, the aqueous layer was extracted with dichloromethane, the combined organic phase was dried with anhydrous sodium sulfate, the solvent was distilled, the silica gel column chromatography (pure petroleum ether) was removed, and the compound a5.24g (22mmol) was obtained by vacuum drying to give compound a5.24g (22mmol), with a yield of 88.1%.
References:
CN113979974,2022,A Location in patent:Paragraph 0008; 0055-0058
585-70-6
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32460-15-4
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2689-65-8
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18614-11-4
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854819-96-8
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18614-11-4
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