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Azobisisobutyronitrile → 2-Bromo-3-phenyl-6-(3-phenylpropoxy)indene-1-one
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-Phenyl-6-(3-phenylpropoxy)indene-1-one | HCID 68694743 | — |
| 触媒 | Tungsten | HCID 23964 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 生成物 | 2-Bromo-3-phenyl-6-(3-phenylpropoxy)indene-1-one | HCID 68695076 | 60% |
反応手順
3-Phenyl-6-(3-phenyl-propoxy)-indene-1-one (200 mg, 0.586 mmol) obtained in Step 1 was dissolved in carbon tetrachloride, and N-bromosuccinimide (313 mg, 1.75 mmol) and 2,2′-azobisisobutyronitrile (9.7 mg) were added thereto. The mixture was refluxed for 1 hr under the irradiation of a 375 W tungsten lamp. Upon the completion of the reaction, the mixture washed with saturated saline and extracted with dichloromethane. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography (ethyl acetate:hexane=1:5) to obtain 147 mg of the titled compound (yield: 60%) as a red solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745439B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-93b0980d393d482f97ea807b4febef77 |
| 出典メモ | uspto-grants-2010_06 |