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Ethyl Acetate → 4,5-Dihydro-1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4-Fluorophenylhydrazine hydrochloride | HCID 69981 | — |
| 反応物 | 3-[4-(Methylthio)phenyl]acrylonitrile | HCID 4239680 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4,5-Dihydro-1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine | HCID 10494529 | 67.6% |
反応手順
4-Fluorophenylhydrazine hydrochloride 4 g) was added to a solution of sodium (1.13 g) in ethanol (50 ml), and the mixture was refluxed for 1 hour. To the cooled mixture was added 3-[4-(methylthio)phenyl]acrylonitrile (4.3 g), and the resulting mixture was refluxed overnight. Ethyl acetate and water were added, and the organic layer was separated, dried and concentrated. The oily residue (7.6 g) was purified by column chromatography on silica gel (76 g) eluting with a mixture of toluene and ethyl acetate (2:1) to give brown crystals of 4,5-dihydro-1-(4-fluorophenyl)-5-[4-(methylthio)phenyl]pyrazol-3-amine (5 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05134142 |
| 出典データセット | uspto-grants-1992_07 |
| ORD ID | ord-2425888f196f492396fa15bd73dac99d |
| 出典メモ | uspto-grants-1992_07 |