Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Iodine | HCID 807 | — |
| Edukt | Thiosulfuric acid, disodium salt, monohydrate | HCID 108762 | — |
| Edukt | 9-Bromo-10-phenyl-anthracene | HCID 4155836 | — |
| Edukt | Butyllithium | HCID 178418339 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| 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 the temperature was lowered to −78° C. 7.5 ml (12.0 mmol) of n-BuLi (1.6M) was dropped into the reaction solution by a dropping funnel, and it was stirred for 1 hour. A solution in which 5 g (20.0 mmol) of iodine was dissolved in 20 ml of THF was dropped and stirred for 2 hours at −78° C. After reaction, a sodium thiosulfate water solution was added to stop the reaction. An organic layer was washed with a sodium thiosulfate water solution and a saturated saline and dried with magnesium sulfate. After the natural filtration, the filtrate was concentrated and the obtained solid was recrystallized by ethanol. Then, 3.1 g of a light-yellow solid of 9-iodo-10-phenylanthracene, which was the intended object, was obtained with a yield of 83% (synthetic scheme of (b-5)).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patentnummer | US08003977B2 |
|---|
| Quelldatensatz | uspto-grants-2011_08 |
|---|
| ORD ID | ord-cbb472fa9b5d4eeeace4a22cc97865e5 |
|---|
| Quellennotiz | uspto-grants-2011_08 |
|---|