関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Dioxide | HCID 280 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2-Bromo-9,9-di-n-octylfluorene | HCID 12964693 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9,9-Dioctyl-9H-fluorene-2-carboxylic Acid | HCID 21982080 | — |
反応手順
Into a flask fitted with a nitrogen inlet and rubber septum were introduced 2-bromo-9,9-dioctylfluorene (34.18 g, 72.8 mmole) and dry tetrahydrofuran (300 mL). The solution was cooled to −60° C. and n-butyl lithium (29.1 mL, 2.5M in hexanes, 72.8 mmole) added via a syringe. The reaction mixture was observed to turn red. After stirring for 1 hour at −60° C., the reaction mixture was poured onto powdered dry-ice and left to stand overnight. The mixture was acidified with 1M HCl and extracted with chloroform. The chloroform extract was washed with water, dried over magnesium sulfate and concentrated to give the acid as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07271406B2 |
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| 出典データセット | uspto-grants-2007_09 |
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| ORD ID | ord-ae374cb4cd624c8caf93abecd566ff53 |
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| 出典メモ | uspto-grants-2007_09 |
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