関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | (2S, 4S)-2-Carbamoyl-4-(4-methoxybenzylthio)-pyrrolidine | HCID 14880267 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (2S, 4S)-2-Carbamoyl-1-ethyl-4-(4-methoxybenzylthio)pyrrolidine | HCID 14796650 | — |
反応手順
0.362 ml of ethyl iodide and 315 mg of sodium bicarbonate to a solution of 1000 mg of (2S, 4S)-2-carbamoyl-4-(4-methoxybenzylthio)pyrrolidine dissolved in 10 ml of dry dimethylformamide were added, whilst ice-cooling, and the mixture was stirred at room temperature for 5.5 hours. At the end of this time, the reaction mixture was poured into a saturated aqueous solution of sodium bicarbonate and extracted with ethyl acetate. The extract was washed with an aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and then the solvent was removed by distillation under reduced pressure. The residue was subjected to column chromatography through silica gel (Katayama Chemicals Co., Silica Gel 60K070) and 560 mg of the title compound were obtained as crystals, melting at 124°-125° C., from the fractions eluted with ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05242914 |
|---|
| 出典データセット | uspto-grants-1993_09 |
|---|
| ORD ID | ord-ad59de36260c4266b878a79c69cfa272 |
|---|
| 出典メモ | uspto-grants-1993_09 |
|---|