化工社化工社 化学情報印刷レポート · 研究参考用
Iodine → 1~4~-Iodo-1~1~,2~1~:2~3~,3~1~-terphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | M-Terphenyl | HCID 7076 | — |
| 反応物 | Hydroiodic acid dihydrate | HCID 85613701 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1~4~-Iodo-1~1~,2~1~:2~3~,3~1~-terphenyl | HCID 12378402 | — |
| 生成物 | 5'-Iodo-m-terphenyl | HCID 13067230 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09139522B2 |
| 出典データセット | uspto-grants-2015_09 |
| ORD ID | ord-a4026af5f96145e1a1263c9b7eb65129 |
| 出典メモ | uspto-grants-2015_09 |