化工社化工社 化学情報印刷レポート · 研究参考用
Nitrogen → 6-Anthracen-9-ylphenanthrene-9-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 6-Bromophenanthrene-9-carboxylic acid | HCID 289464 | — |
| 反応物 | 9-Anthraceneboronic Acid | HCID 15510213 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Methanol--water (1/1) | HCID 22242641 | — |
| 生成物 | 6-Anthracen-9-ylphenanthrene-9-carboxylic acid | HCID 59629491 | — |
反応手順
32.86 g (148 mmol) of anthracene-9-boronic acid, 37.2 g (124 mmol) of 6-bromophenanthrene-9-carboxylic acid and 220 ml of 2 M Na2CO3 solution are suspended in 1 l of toluene and 1 l of EtOH, the mixture is saturated with N2, 2.9 g (3 mmol) of tetrakis(triphenylphosphine)palladium(0) are added, and the mixture is heated at the boil for 2 h. The mixture is poured into 3 l of a mixture of water/MeOH/6 M HCl 1:1:1, and the beige precipitate is filtered off with suction, washed with water, EtOH and toluene and dried. The content of product according to 1H-NMR is about 96% with an overall yield of 38.5 g (78%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08993123B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-3ebbd0e323584a6d9b3fabd3922fed03 |
| 出典メモ | uspto-grants-2015_03 |