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Ethanol → ethyl 5-chloro-3-(trifluoromethyl)-1H-pyrazole-1-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Acetic acid, 2-hydrazinyl-, ethyl ester, hydrochloride (1:1) | HCID 11593468 | — |
| 反応物 | 1,1,1-Trifluoro-4,4-dichloro-3-buten-2-one | HCID 15548324 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | ethyl 5-chloro-3-(trifluoromethyl)-1H-pyrazole-1-acetate | HCID 66016896 | — |
反応手順
To a mixture of ethyl hydrazinoacetate hydrochloride (2.8 g, 18.1 mmol) and triethylamine (9.2 g, 91 mmol) in a solution of ethanol (20 mL) and N,N-dimethylformamide (1 mL), a solution of crude 4,4-dichloro-1,1,1-trifluoro-3-buten-2-one in dichloromethane (20 mL) was added dropwise while keeping the temperature of the reaction mixture below 10° C. After stirring a further 2 h at below 10° C., the reaction mixture was concentrated under reduced pressure. The residue was diluted with diethyl ether, and the mixture was filtered. The resulting filtrate was concentrated to give 4.34 g of the title compound as a solid. This compound was of sufficient purity to use in subsequent reactions.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08642634B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-88a7200bbf6c40a79c4d74d69d6dba68 |
| 出典メモ | uspto-grants-2014_02 |