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HRID 900392作成日:2026年10月26日

Water → Ethyl 1-(2,4-dichlorophenyl)-4-methyl-5-oxo-4,5-dihydro-1H-pyrazole-3-carboxylate

https://huagongshe.com/reaction/900392

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Trifluoroacetic acidHCID 6422—
反応物Butanedioic acid, 2-methyl-3-oxo-, 1,4-diethyl esterHCID 97750—
反応物(2,4-Dichlorophenyl)hydrazine monohydrochlorideHCID 2723905—
溶媒TolueneHCID 1140—
生成物Ethyl 1-(2,4-dichlorophenyl)-4-methyl-5-oxo-4,5-dihydro-1H-pyrazole-3-carboxylateHCID 86760639—

反応条件

温度75 °C

反応手順

2,4-dichlorophenylhydrazine hydrochloride(12.6 g) is dissolved in 100 ml of toluene and this solution is placed under nitrogen; after stirring, 10 g of diethyl 2-methyl-3-oxosuccinate are added and the mixture is then heated and 5 ml of TFA are added at 55° C. The mixture is left at the reflux of the solvent for 4 and a half hours, with stirring. The mixture is allowed to return to ambient temperature and is then heated to 75° C. and the reaction medium is hydrolyzed with 30 ml of water. The mixture is separated by settling out, the aqueous phase is discarded and the organic phase is then evaporated in order to eliminate the residual TFA. The organic phase is taken up with 10 ml of toluene and the expected product then crystallizes, m=10.2 g.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07358371B2
出典データセットuspto-grants-2008_04
ORD IDord-abe29720067d431584a668e3a7708b84
出典メモuspto-grants-2008_04