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p-Bromoacetophenone → 4-Bromo-1-(1,3-dithian-2-yl)ethylbenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Bromoacetophenone | HCID 7466 | — |
| 反応物 | Boron trifluoride etherate | HCID 8000 | — |
| 反応物 | 1,3-Propanedithiol | HCID 8013 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Bromo-1-(1,3-dithian-2-yl)ethylbenzene | HCID 21960112 | — |
反応手順
To the compound p-bromoacetophenone (36.85 g, 185 mmol) in trichloromethane (300 ml) was added 1,3-propanedithiol (25 g, 230 mmol) and boron trifluoride etherate (3 ml). The resulting mixture was stirred at room temperature for 48 hours. The mixture was diluted with dichloromethane (500 ml), washed twice with 10% sodium hydroxide (200 ml), water, and brine, and then dried (Na2SO4). The product was concentrated to an oil. A portion was stirred with ether (100 ml) and a crystalline product was formed. The crystalline product was recovered by filtration and purified by recrystallization to yield 4-bromo-1-(1,3-dithian-2-yl)ethylbenzene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05597842 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-502ee71b6a37491eaa78a96c66ddffb0 |
| 出典メモ | uspto-grants-1997_01 |