化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 1-(2-Bromo-5-chlorophenyl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Bromo-5-chloro-N-methoxy-N-methylbenzamide | HCID 22236546 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Tetrahydrofuran toluene | HCID 22635083 | — |
| 生成物 | 1-(2-Bromo-5-chlorophenyl)ethanone | HCID 12486617 | — |
反応手順
Methylmagnesium bromide (4.26 mL of a 1.4M solution in tetrahydrofuran/toluene, 5.97 mmol) was added dropwise to a stirred solution of 2-bromo-5-chloro-N-methoxy-N-methylbenzamide (3-1) (0.554 g, 1.99 mmol) in tetrahydrofuran (20 mL) at approximately 0° C. After 1 h, 1N hydrochloric acid (5 mL) was added and the resulting biphasic mixture was stirred vigorously for about 10 min. The reaction mixture was poured into water and extracted three times with ethyl acetate. The combined organic extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. Purification of the crude residue by flash chromatography on silica gel (gradient elution; 0-10% ethyl acetate/hexanes as eluent) provided 3-3 (0.44 g) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06818658B2 |
| 出典データセット | uspto-grants-2004_11 |
| ORD ID | ord-994732bb6d2942fbb576ed31e579f72d |
| 出典メモ | uspto-grants-2004_11 |