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Ethanol → 4-(7-Phenylbenz[a]anthracen-4-yl)-7-phenylbenz[a]anthracene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Phenylboronic Acid | HCID 66827 | — |
| 反応物 | N-bromobutanimide | HCID 67184 | — |
| 反応物 | 4-(Benz[a]anthracen-4-yl)benz[a]anthracene | HCID 59412552 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(7-Phenylbenz[a]anthracen-4-yl)-7-phenylbenz[a]anthracene | HCID 59412710 | — |
反応手順
19.6 g (110 mmol) of N-bromosuccinimide are added in one portion at 100° C. with vigorous stirring to a suspension of 22.7 g (50 mmol) of 4-(benz[a]anthracen-4-yl)benz[a]anthracene in 1000 ml of DMF. The suspension is kept at 100° C. for a further 30 min. and cooled, and 1000 ml of ethanol are then added. The precipitated solid is filtered off with suction, washed three times with 100 ml of ethanol each time and dried in vacuo. The resultant solid is reacted analogously to Example 7 with 15.9 g (130 mmol) of benzeneboronic acid, Recrystallisation five times from DMF (about 6 ml/g); sublimation (p=5×10−5 mbar, T=360° C.). Yield: 21.8 g (36 mmol), 72.0%, purity 99.9% (HPLC), Tg=181.4° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08986852B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-52646a4582bf43ba9c9fb5c133992734 |
| 出典メモ | uspto-grants-2015_03 |