関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Triphenylene | HCID 9170 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzene, 1,3-diiodo- | HCID 12270 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1,3-Bis(triphenylen-2-yl)benzene | HCID 58769446 | — |
反応手順
1.23 g (3.5 mmol) of the triphenylene moronic ester from the previous step, 0.5 g (1.5 mmol) of 1,3-diiodobenzene, 1.0 g (7.5 mmol) of potassium carbonate, 30 mL of toluene, and 10 mL of water was mixed in a 250 mL three-neck flask. The system was purged by nitrogen for 10 min before adding 0.05 g of Pd(PPh3)4. The mixture was then heated up to 87° C. with vigorous stirring. After 24 hr, to the mixture was added 200 mL of methanol. The precipitate was collected by filtration. The solid was washed with copious amount of methanol, then hexanes. The solid was then recrystallized from 80 ml of xylenes. Final purification of the product involved subliming the material at 250° C. 0.35 g product was collected as white needle crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08092924B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-08cdd25534ec478b9be339a85721ed6d |
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| 出典メモ | uspto-grants-2012_01 |
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