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Sodium Iodide → HCID 178466792、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | 4'-Hydroxyacetophenone | HCID 7469 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-(2-chloroethyl)-1H-imidazole hydrochloride | HCID 178478570 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 178466792 | HCID 178466792 | — |
反応手順
816 mg (6 mmol) of 4-hydroxyacetophenone, 251 mg (1.5 mmol) of 4-[2-chloroethyl]-1H-imidazole hydrochloride, 500 mg (3.6 mmol) of potassium carbonate and sodium iodide (catalyst) are stirred at 80° C. for 5 days in 5 ml of dimethylformamide. The reaction mixture is cooled, filtered and the filtrate is evaporated under reduced pressure to give an oily residue, from which 4-hydroxyacetophenone is extracted with ether at pH=1. Subsequent extraction with ethyl acetate at pH=9 gives the title compound. The latter was treated with oxalic acid in 2-propanol to give the oxalate of the title compound which is crystallized from a methanol/ether (10/1) mixture, M.p.: 178°-182° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05708171 |
| 出典データセット | uspto-grants-1998_01 |
| ORD ID | ord-33222d5c3e74477ea5aecbacd88d0902 |
| 出典メモ | uspto-grants-1998_01 |