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Nitrogen → 6-(10-Naphthalen-2-ylanthracen-9-yl)phenanthrene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Methanol--water (1/1) | HCID 22242641 | — |
| 反応物 | 6-(10-Naphth-2-ylanthracen-9-yl)phenanthrene-9-carboxylic acid | HCID 59629487 | — |
| 触媒 | HCID 178505374 | HCID 178505374 | — |
| 溶媒 | Quinoline | HCID 7047 | — |
| 生成物 | 6-(10-Naphthalen-2-ylanthracen-9-yl)phenanthrene | HCID 58194430 | — |
反応手順
49 g (94 mmol) of 6-(10-naphth-2-ylanthracen-9-yl)phenanthrene-9-carboxylic acid are suspended in 250 ml of quinoline, the suspension is saturated with N2, 11.8 g (38 mmol) of copper chromite are added, and the mixture is heated at the boil for 8 h. The mixture is subsequently poured into 1 l of MeOH/water, and the black solid is filtered off with suction, washed with MeOH and subjected to Soxhlet extraction with CHCl3. Removal of the solvent leaves a greyish solid, which is recrystallised four times from chlorobenzene and sublimed twice in vacuo (p=1×10−5 mbar, T=360° C.). The yield is 32 g (71%) with a purity>99.9%.
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-aad495be30e24421a7bc140a5134821f |
| 出典メモ | uspto-grants-2015_03 |