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Dichloroacetyl chloride → ST50911991
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloroacetyl chloride | HCID 6593 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(4-Nitrophenyl)piperazine | HCID 80447 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | ST50911991 | HCID 2837846 | 46% |
反応手順
7.1 g (0.048 mol) of dichloroacetyl chloride were added dropwise to a solution of 10 g (0.048 mol) of 1-(4-nitrophenyl)-piperazine and 5 g (0.495 mol) of triethylamine in 100 ml of toluene at room temperature, while stirring. The mixture was subsequently stirred at 20° C. for 3 hours. Working up was then effected by a procedure in which the reaction mixture was washed twice with 100 ml of water each time and the organic phase was separated off, dried and evaporated under reduced pressure. The residue was recrystallized from toluene. 7 g (46% of theory) of 1-(4-nitrophenyl)-4-dichloroacetyl-piperazine were obtained in the form of light yellow crystals of melting point 155° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04422866 |
| 出典データセット | uspto-grants-1983_12 |
| ORD ID | ord-a2ca27a80e8c43d2b6bf33d8d91bd5aa |
| 出典メモ | uspto-grants-1983_12 |