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Sodium Azide → 3-Bromophenacyl azide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Azide | HCID 33557 | — |
| 反応物 | 2-Bromo-1-(3-bromophenyl)ethan-1-one | HCID 519585 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Bromophenacyl azide | HCID 16748734 | 99.3% |
反応手順
A solution of 20.2 g (73 mmol) of 3-bromophenacyl bromide and 5.42 g (83 mmol) of sodium azide was stirred at RT for 90 min in methanol. The solvent was removed under reduced pressure and the crude product was partitioned between ethyl acetate (200 ml) and water (100 mL). The organic layer was separated, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to afford the title compound (17.4 g, 99%) as a light yellow solid. 1H NMR (400 MHz, d6-DMSO): δ 8.10 (d, J=1.0, 1H), 7.90–7.97 (m, 2H), 7.22 (t, J=7.9, 1H), 4.93 (s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07189712B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-04496d367c7b4f678864836d4b3ee3b1 |
| 出典メモ | uspto-grants-2007_03 |