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4-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotoluene → 1-Hydroxy-6-(trifluoromethyl)benzotriazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotoluene | HCID 8462 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-Hydroxy-6-(trifluoromethyl)benzotriazole | HCID 688194 | 89.5% |
反応手順
The title compound is prepared according to the procedure described by K. Takeda [J. Org. Chem., 50, 273, (1985)]. A mixture of 4-chloro-3-nitro-α,α,α-trifluorotoluene (50.0 g, 0.22 moles) and hydrazine hydrate (33.0, 0.33 moles) in absolute ethanol (75 ml) is refluxed for 24 h. After removal of the solvent under reduced pressure, the residue is dissolved in 10% aqueous sodium carbonate solution. The solution is washed with ether to remove the starting material and acidified with concentrated HCl to precipitate the product, which is washed with water and dried to obtain 40.0 g of the title compound. This product is recrystallized from ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094872B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-868789ba44d24a379570d31b85128dc2 |
| 出典メモ | uspto-grants-2006_08 |