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1-Bromopropane → 5-Nitro-1-propylindoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Bromopropane | HCID 7840 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 5-Nitroindoline | HCID 36219 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-Nitro-1-propylindoline | HCID 9834276 | — |
反応手順
0.51 g (12.79 mmoles) of 60% NaH is added, at 20° C., by portions, to a solution of 2 g (12.18 mmoles) of 5-nitroindoline in 16 ml of anhydrous DMF. After stirring for a further 30 minutes, 2.32 ml (25.58 mmoles) of 1-bromopropane is added dropwise. Stirring is maintained overnight and the reaction mixture is finally diluted with 50 ml of water and 50 ml of AcOEt. After stirring and decanting, the organic phase is successively washed with 25 ml of water and 25 ml of salt water, dried over Na2SO4, filtered and concentrated to dryness under vacuum. The evaporation residue is then purified on a silica column (eluent: Heptane/AcOEt: 9/1). Orange oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06747024B1 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-796e6a3fb63845a989e31572ba112b64 |
| 出典メモ | uspto-grants-2004_06 |