関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Azobisisobutyronitrile | HCID 6547 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 3-Bromo-4-methylbenzoic acid | HCID 82130 | — |
| 溶媒 | (Trifluoromethyl)benzene | HCID 7368 | — |
| 生成物 | 3-bromo-4-(bromomethyl)benzoic Acid | HCID 11616314 | 60% |
反応手順
To a solution of 3-bromo-4-methylbenzoic acid (1.0 equiv.) and AIBN (0.05 equiv.) in trifluorotoluene (0.28 M) was added NBS (1.1 equiv.). The mixture was heated at 90° C. overnight. The reaction mixture was partitioned between EtOAc and H2O. The organic layer was washed with NaCl(sat.), dried over MgSO4, filtered, concentrated to yield 3-bromo-4-(bromomethyl)benzoic acid in 60% yield. LC/MS (m/z)=294.8 (MH+), Rt=0.80 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09242969B2 |
|---|
| 出典データセット | uspto-grants-2016_01 |
|---|
| ORD ID | ord-a5833216af294f4aa238714c4ebbf9dd |
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| 出典メモ | uspto-grants-2016_01 |
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