Methyl arylpyrazole fluorouracil compounds, and preparation method and application thereof
A compound, pyridine technology, applied in the field of pesticides, achieves the effects of simple synthesis process, less residue in the body, and fast metabolism
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Embodiment 1
[0058] This example illustrates the synthesis of 5-fluorouracil acetic acid
[0059] Add KOH1.12g (20mmol), H 2 O15mL, after dissolving, add 2.6g (20mmol) of 5-fluorouracil (20mmol) and 1.82g (22mmol) of chloroacetic acid in 10mL aqueous solution, and continue the reaction for 6h after completion. After the reaction, the pH was adjusted to 2 with concentrated hydrochloric acid, a large amount of white solid precipitated, filtered, washed with water, and recrystallized with water to obtain 3.0 g of the product with a yield of 80%. Product melting point: 289-291°C.
Embodiment 2
[0061] This example illustrates the synthesis of 5-fluorouracil amidoalcohol
[0062] Add 3.76 g (20 mmol) of 5-fluorouracil acetic acid into a three-necked flask, dissolve it in 50 mL of DMF, and stir for 1 h. At room temperature, 1.6 g (24 mmol) of ethanolamine was slowly added dropwise, and the reaction was refluxed for 24 h. After the reaction was completed, 100 mL of water was added after concentrating the solvent, a large amount of solids precipitated, filtered, washed with water, and recrystallized with ethanol to obtain 3.18 g of the product, with a yield of 69%. Product melting point: 253-256°C.
Embodiment 3
[0064] This example illustrates the synthesis of 3-methyl-1-phenyl-1H-pyrazole-5-carboxylic acid
[0065] Add 10mmol of phenylhydrazine and 15ml of ethanol to a four-neck flask, dissolve and add 1.58g (10mmol) of ethyl acetylacetonate, react at room temperature for 2h, filter, and recrystallize from ethanol to obtain 5-hydroxy-3-methyl-1-phenyl -4,5-Dihydro-1H-pyrazole-5-carboxylic acid ethyl ester.
[0066] Add the above product and 8ml of concentrated hydrochloric acid into a four-necked flask, and heat to reflux for 2h. After the reaction, the solvent was spin-dried to obtain ethyl 3-methyl-1-phenyl-1H-pyrazole-5-carboxylate.
[0067] Add the above product and 20ml of 50% NaOH into a four-necked flask, and heat to reflux for 2h. After the reaction, cool to room temperature, adjust the pH to 2-3 with concentrated hydrochloric acid, extract with ethyl acetate, take the organic phase, dry, rotary evaporate, and recrystallize to obtain a white solid. The yield is 58.2%, and ...
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