関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Dibromobenzene | HCID 7927 | — |
| 反応物 | Bromhydrol | HCID 166749 | — |
| 反応物 | 3,3'-Dibromo-5,5',7,7'-tetramethyl-1,1'-biadamantane | HCID 57934707 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 生成物 | 3,3',5,5'-Tetramethyl-7,7'-bis(3,5-dibromophenyl)-1,1'-biadamantane | HCID 57558380 | 180% |
反応手順
A 3-liter recovery flask was charged with the above synthesized 7,7′-dibromo-3,3′,5,5′-tetramethyl-1,1′-biadamantane 48.4 g (100 mmol), 1,3-dibromo benzene 1180 g (500 mmol), and a stirrer. While stirring under a nitrogen flow at room temperature, aluminum bromide (III) 26.7 g (100 mmol) was added little by little. After the end of addition, the solution was stirred at 50° C. for 7 hours. The reaction solution was charged into a 1 mol/liter hydrochloric acid solution 2 liter, the aqueous phase was removed by separation, then acetone 1 liter was added for extraction. The solid was collected by filtration and dried under reduced pressure to obtain 7,7′-bis(3,5-dibromophenyl)-3,3′,5,5′-tetramethyl-1,1′-biadamantane (90.0 mmol; yield 90.0%) 71.5 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08530596B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-482d535ef50f4cb0ae074e5269c7e9b0 |
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| 出典メモ | uspto-grants-2013_09 |
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