化工社化工社 化学情報印刷レポート · 研究参考用
Acetic Acid → 2-Bromodibenzofuran
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Dibenzofuran | HCID 568 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Bromodibenzofuran | HCID 6856 | 31% |
反応手順
150 g of dibenzofuran (892 millimoles) and 1 liter of acetic acid were placed in a flask, which was then replaced with nitrogen and the contents of which were dissolved under heating. After 188 g of bromine (1.18 moles) were dropped while being occasionally cooled with water, the mixture was stirred for 20 hours under cooling with air. The precipitated crystals were filtrated, washed sequentially with acetic acid and water, and dried under reduced pressure. After the crystals obtained were purified by distillation under reduced pressure, recrystallization from methanol was performed several times to obtain 66.8 g of 2-bromodibenzofuran (yield 31%). The resultant was identified as Intermediate 4 by FD-MS analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09382206B2 |
| 出典データセット | uspto-grants-2016_07 |
| ORD ID | ord-285b2d99a93a478ba3a119d70c072aa4 |
| 出典メモ | uspto-grants-2016_07 |