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Hydrochloric Acid → (5-Bromo-2-chlorophenyl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Diisobutylaluminum hydride | HCID 14487 | — |
| 反応物 | Methyl 5-bromo-2-chlorobenzoate | HCID 842098 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (5-Bromo-2-chlorophenyl)methanol | HCID 5074766 | 93.7% |
反応手順
25.0 g of methyl 5-bromo-2-chlorobenzoate was dissolved in 130 ml of dichloromethane. To this solution, 230 ml of a 0.96 M DIBAL (diisobutylalminium hydride) hexane solution was added at −40° C. in a nitrogen atmosphere, followed by stirring at room temperature for 4 hours. To this reaction solution, 10% hydrochloric acid was carefully added while cooling, followed by extraction with ethyl acetate and drying over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the obtained crude crystals were washed with hexane to obtain 20.8 g of 5-bromo-2-chlorobenzyl alcohol as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06313071B1 |
| 出典データセット | uspto-grants-2001_11 |
| ORD ID | ord-07e2e2f8419c4e1585ce0de5e3e8845e |
| 出典メモ | uspto-grants-2001_11 |