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Benzoyl Peroxide → 4-(Benzhydrylidene-amino)-3-bromomethyl-benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoyl Peroxide | HCID 7187 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 4-(Benzhydrylidene-amino)-3-methyl-benzonitrile | HCID 19350962 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(Benzhydrylidene-amino)-3-bromomethyl-benzonitrile | HCID 10499686 | 56.9% |
反応手順
To a solution of 4-(benzhydrylidene-amino)-3-methyl-benzonitrile (1.36 g, 4.27 mmol) in 40 mL of CCl4 is added N-bromosuccinimide (0.84 g, 4.7 mmol) and benzoyl peroxide (0.22 g, 0.64 mmol). The solution is heated to reflux for 16 h. The solution is cooled to ambient temperatures. The solution is diluted with CH2Cl2. The solution is washed with 1N NaOH and saturated NaCl. The organic layer is dried over MgSO4, filtered and concentrated. The crude material is purified by column chromatography eluting with a gradient of 5% EtOAc/hexanes to 10% EtOAc/hexanes. The title compound (0.91 g, 2.43 mmol) is obtained as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05731315 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-d5d7a05761ee49b4bed0ffdf724b4bc7 |
| 出典メモ | uspto-grants-1998_03 |