HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Iodine → 1~4~-Iodo-1~1~,2~1~:2~3~,3~1~-terphenyl
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Iodine | HCID 807 | — |
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | M-Terphenyl | HCID 7076 | — |
| Edukt | Hydroiodic acid dihydrate | HCID 85613701 | — |
| Lösungsmittel | Acetic Acid | HCID 176 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | 1~4~-Iodo-1~1~,2~1~:2~3~,3~1~-terphenyl | HCID 12378402 | — |
| Produkt | 5'-Iodo-m-terphenyl | HCID 13067230 | — |
Reaktionsschritte
A three-necked flask was charged with 250 g of m-terphenyl (ALDRICH), 50 g of hydroiodic acid dihydrate, 75 g of iodine, 750 ml of acetic acid, and 25 ml of concentrated sulfuric acid, and reaction was allowed to proceed at 70° C. for 3 hours. The product was poured into 5 L of methanol and the mixture was stirred for 1 hour and filtrated. The obtained crystals were purified by column chromatography, and recrystallized from acetonitrile to give 64 g of 3′-phenyl-4-iodobiphenyl (Intermediate 4) and 17 g of 3-phenyl-5-iodobiphenyl in the form of white powder. FD-MS and H-NMR analysis identified the powder as Intermediate 4.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09139522B2 |
| Quelldatensatz | uspto-grants-2015_09 |
| ORD ID | ord-a4026af5f96145e1a1263c9b7eb65129 |
| Quellennotiz | uspto-grants-2015_09 |