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(4-Methylphenyl)hydrazine → 4,5-dihydro-1-(4-methylphenyl]-5-(4-methylsulphonylphenyl)-3-trifluoromethyl-1H-pyrazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (4-Methylphenyl)hydrazine | HCID 10875 | — |
| 反応物 | (E)-1,1,1-trifluoro-4-(4-methylsulphonylphenyl)-3-butene-2-one | HCID 15484796 | — |
| 触媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4,5-dihydro-1-(4-methylphenyl]-5-(4-methylsulphonylphenyl)-3-trifluoromethyl-1H-pyrazole | HCID 9929869 | 32% |
反応手順
In a flask with an inert atmosphere (E)-1,1,1-trifluoro-4-(4-methylsulphonylphenyl)-3-butene-2-one (prepared according to the method E-1) (1.83 g, 6.58 mmoles) and 4-methylphenylhydrazine chlorohydrate (1.04 g, 6.58 mmoles) are dissolved in 50 ml de ethanol. A few drops of hydrochloric acid are added, and the mixture refluxed under an inert atmosphere for 4 days. The mixture is cooled and the product crystallised. The solution is filtered and the product recrystallised from ethanol. 4,5-dihydro-1-(4-methylphenyl]-5-(4-methylsulphonylphenyl)-3-trifluoromethyl-1H-pyrazole (0.8 g, yield: 32%) is obtained in the form of a solid with a melting point of 140-3° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06353117B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-64c3958b6e4247e4815fd2db1550476b |
| 出典メモ | uspto-grants-2002_03 |