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Sodium Iodide → HCID 178469080、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 | Ethylparaben | HCID 8434 | — |
| 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 178469080 | HCID 178469080 | — |
反応手順
1.49 g (9 mmol) of ethyl 4-hydroxybenzoate, 251 mg (1.5 mmol) of 4-(2-chloroethyl)-1H-imidazole hydrochloride, 500 g (3.6 mmol) of potassium carbonate and sodium iodide (catalyst) are stirred at 80° C. for 4 days in 5 ml of dimethylformamide. The reaction mixture is cooled and then filtered. The filtrate is evaporated under reduced pressure to give an oily residue. The excess ethyl 4-hydroxybenzoate is extracted with ether at pH=1. The aqueous solution is evaporated under reduced pressure to give the title compound. The latter is purified by preparative high performance chromatography and converted to the oxalate which, after crystallization from an isopropanol/ether mixture, melts at 160°-164° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05559113 |
| 出典データセット | uspto-grants-1996_09 |
| ORD ID | ord-37b947fe38e748aca21ed87b467e4b05 |
| 出典メモ | uspto-grants-1996_09 |