関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | 4-Hydroxybiphenyl | HCID 7103 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | sodium thiosulfite anhydrous | HCID 15847209 | — |
| 反応物 | Sodium Hypochlorite | HCID 23665760 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-Hydroxy-3-iodobiphenyl | HCID 4106140 | — |
反応手順
Biphenyl-4-ol((5.26 g, 30.9 mmol), sodium iodide (4.635 g, 30.9 mmol), sodium hydroxide (1.276 g, 31.9 mmol) was dissolved in methanol (85 mL) and cooled to 0° C. To the solution was added 12% (w/v) sodium hypochlorite (20 mL) dropwise maintaining the temperature below 4° C. The solution was stirred at this temperature for 1 hour and then 2M sodium thiosulfite (50 mL) wad added and the pH of the solution was adjusted to >pH 7 with 1M HCl. The mixture was filtered and the filtrate was washed with water. The solid was dried in a vacuum oven and then the title product was obtained as crystals after recrystallisation from heptane. Yield 7.08 g, 77%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07612068B2 |
|---|
| 出典データセット | uspto-grants-2009_11 |
|---|
| ORD ID | ord-015dc7f31fe34963ae9cf14d583f1eee |
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| 出典メモ | uspto-grants-2009_11 |
|---|
