Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Iodine | HCID 807 | — |
| Edukt | Sodium Thiosulfate | HCID 24477 | — |
| Edukt | 9-Bromo-10-phenyl-anthracene | HCID 4155836 | — |
| Edukt | Butyllithium | HCID 178418339 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Lösungsmittel | Hexane | HCID 8058 | — |
| Produkt | 9-Iodo-10-phenylanthracene | HCID 14958373 | 83% |
Reaktionsschritte
3.33 g (10 mmol) of 9-bromo-10-phenylanthracene was dissolved in 80 mL of tetrahydrofuran (abbreviation: THF), and cooled to −78° C. Then, in a reaction solution thereof, 7.5 mL (12.0 mmol) of n-buthyllithium (abbreviation: n-BuLi) (1.6 mol/L hexane solution) was dropped by a dropping funnel and then stirred for one hour. A solution in which 5 g (20.0 mmol) of iodine dissolved in 20 mL of THF was dropped therein, and the further stirred for 2 hours at −78° C. After reaction, a sodium thiosulfate aqueous solution was added therein and stirred. An organic layer was washed with a sodium thiosulfate aqueous solution and saturated saline, and then dried with magnesium sulfate. The mixture was filtrated naturally, then the filtrate was concentrated, and then recrystallized with ethanol, 3.1 g of 9-iodo-10-phenylanthracene that was a target substance was obtained as a light yellow solid at a yield of 83% (Synthesis scheme (b-3)).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08860019B2 |
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| Quelldatensatz | uspto-grants-2014_10 |
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| ORD ID | ord-c5def690792e40f1b745718d1ddb34ce |
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| Quellennotiz | uspto-grants-2014_10 |
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