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1,3-Dibromopropane → HCID 58097204、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,3-Dibromopropane | HCID 8001 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3,6-Dibromocarbazole | HCID 274874 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 58097204 | HCID 58097204 | 28.6% |
反応手順
Crushed KOH (0.0673 g, 1.20 mmol, 1.2 equiv) was added to 3,6-dibromocarbazole (0.3250 g, 1.00 mmol) in 2 mL DMF solution and the mixture was stirred for 30 min. 1,3-dibromopropane (0.5047 g, 2.50 mmol, 2.5 equiv) in 3 mL DMF solution was added dropwise into the mixture and it was stirred at room temperature overnight. The crude reaction mixture was diluted with 30 mL EtOAc and washed with 1M HCl 2×10 mL and water 3×10 mL. The organic layer was dried over anhydrous Na2SO4 and evaporated to afford the crude product, which was subjected to silica gel chromatography using Hexanes/EtOAc to afford 0.1275 g colorless oil as product, yield 28.6%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09446022B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-8148a197ba224f0199ad9a7179b4cc06 |
| 出典メモ | uspto-grants-2016_09 |