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2,2,2-Trifluoroethanol → 4-Chloro-2-nitro-5-(2,2,2-trifluoroethyloxy)toluene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 反応物 | 1,2-Dichloro-4-methyl-5-nitrobenzene | HCID 343795 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 生成物 | 4-Chloro-2-nitro-5-(2,2,2-trifluoroethyloxy)toluene | HCID 19692322 | — |
反応手順
40.4 g (360 mmol) of potassium tert-butylate were added in portions to 60 ml of trifluoroethanol, while stirring and cooling, and the mixture was heated to 80°-90° C. After cooling, 14.4 g (70 mmol) of 4,5-dichloro-2-nitrotoluene were added and the mixture was stirred at 105° C. for 1 hour. It was concentrated in vacuo and the residue was treated with 300 ml of water to give, after filtration with suction, 12 g of crude product, which were purified over silica gel with n-heptane/ethyl acetate, 10 g of product, melting point 76°-79° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726305 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-5c297b4a87b04776a1276a465dc94abc |
| 出典メモ | uspto-grants-1998_03 |