関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | 4-Bromoanisole | HCID 7730 | — |
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 生成物 | HCID 178418276 | HCID 178418276 | — |
反応手順
Magnesium (36 g, 1.5 mol), iodine (a few crystals) and THF (1 L) were heated under nitrogen, with stirring, at reflux for 15 min. The mixture was cooled to 20° C., stirring stopped, and 1,2-dibromoethane (2.5 ml) added. After an exothermic reaction was observed (a few min) stirring was restarted which was accompanied by a rise in temperature to 35° C. The mixture was cooled to 20° C. and 4-bromoanisole slowly added over 1 h at 14°-18° C. with cooling. Stirring was continued for 10 min after the addition was complete.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05726315 |
|---|
| 出典データセット | uspto-grants-1998_03 |
|---|
| ORD ID | ord-f12406699295447fa245b2a1d83d7703 |
|---|
| 出典メモ | uspto-grants-1998_03 |
|---|
