関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Trimethylsilyl cyanide | HCID 82115 | — |
| 反応物 | 2-(4-Phenoxyphenyl)-1-phenyl-1-ethanone | HCID 2824056 | — |
| 触媒 | Magnesium diiodide | HCID 5462737 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-2-(4-phenoxyphenyl)propionitrile | HCID 12056390 | — |
反応手順
A mixture of 4-phenoxyphenylacetophenone (6.36 g), trimethylsilylcyanide (3.96 g) and magnesium iodide (10 mg) in methylene chloride (30 ml) was stirred for 12 hrs at room temperature, 15% hydrochloric acid (10 ml) was then added. The mixture was again stirred for 8 hrs at room temperature. The organic layer was separated and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure. The residue was dissolved in benzene (50 ml) and pyridine (2.37 g) and thionyl chloride (4.76 g) were added at 0° C. with stirring. The reaction mixture was stirred for an additional 3 hrs at room temperature and then the solvent was evaporated. The residue was purified by column chromatography to give 7.09 g of 2-chloro-2-(4-phenoxyphenyl)propionitrile as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06713629B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-ff306ddd6e434acab73221100de33b89 |
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| 出典メモ | uspto-grants-2004_03 |
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