関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | 2,6-Di-tert-butylphenol | HCID 31405 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3',5'-Bis(tert-butyl)-4'-hydroxyacetophenone | HCID 616296 | — |
反応手順
Under a nitrogen atmosphere, 6.89 ml of acetylchloride and 14.75 ml of stannic chloride were dissolved in 200 ml of methylene chloride and chilled to -4° C. To this was added 20 g of 2,6-di-t-butylphenol (in 100 ml of methylene chloride) over 10 minutes. The resultant mixture was stirred for 30 minutes at 0° C., then poured into a mixture of 400 ml of ice and 1N hydrochloric acid and stirred. The mixture separated into layers which were subsequently separated. The organic layer was washed with 100 ml of saturated sodium bicarbonate and 100 ml of brine. The organic layer was dried and the solvent evaporated to give 23.39 g of the desired subtitled intermediate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05731336 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-5ea8ac69bd1848ae813a64e74a7a7adf |
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| 出典メモ | uspto-grants-1998_03 |
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