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Hydrochloric Acid → 3,3',5,5'-Tetramethyl-7,7'-bis(3,5-dibromophenyl)-1,1'-biadamantane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 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 | — |
| 生成物 | 3,3',5,5'-Tetramethyl-7,7'-bis(3,5-dibromophenyl)-1,1'-biadamantane | HCID 57558380 | 180% |
反応手順
In a 1 L recovery flask, 48.4 g of 7,7′-dibromo-3,3′,5,5′-tetramethyl-1,1′-biadamantane (100 mmol), 1,180 g of 1,3-dibromobenzene (5.00 mol) and a stirrer were charged. Under nitrogen flow, 26.7 g of aluminum bromide (100 mmol) was gradually added thereto with agitating at room temperature. After the addition, the mixture was agitated at 50° C. for seven hours. Reaction solution was added to 2 L of 1 mol/L hydrochloric acid aqueous solution. After an aqueous layer was separated and removed therefrom, 1 L of acetone was added. Solid thus precipitated was collected by filtration and dried under reduced pressure, thus obtaining 71.5 g of 7,7′-bis(3,5-dibromophenyl)-3,3′,5,5′-tetramethyl-1,1′-biadamantane (90.0 mmol; yield: 90.0%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07863347B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-a5434d3484454dacb04ccc5387732d5c |
| 出典メモ | uspto-grants-2011_01 |