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Sodium Hydroxide → N-isobutyl-3-bromopyrrolidine-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | rac-2,4-Dibromo-N-isobutyl-butyramide | HCID 53701208 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-isobutyl-3-bromopyrrolidine-2-one | HCID 23303156 | — |
反応手順
4.48 g (14.9 mmol) rac-2,4-Dibromo-N-isobutyl-butyramide were dissolved in 40 ml dichloromethane, then 17.3 ml of 50% sodium hydroxide solution and 0.48 g Dowex 2×10 were added. The mixture was stirred vigorously for 4 h at room temperature. Afterwards the mixture was poured into 50 ml ice/water an the phases were separated. The aqueous phase was extracted thrice with 20 ml dichloromethane, and the combined organic phases were washed once with 20 ml water, once with 20 ml brine and dried over magnesium sulfate. After evaporation of the solvent, the resulting colourless oil was chromatographed or silica gel (0.040-0.063 mm) with ethyl acetate/n-hexane 1:1 as eluent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05925632 |
| 出典データセット | uspto-grants-1999_07 |
| ORD ID | ord-f76b08f8a5e247dca48a9237a7c4d875 |
| 出典メモ | uspto-grants-1999_07 |