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Water → 1-Bromo-4-methoxy-2-(methylsulfonyl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | 1-Methoxy-3-(methylsulfonyl)benzene | HCID 259650 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-Bromo-4-methoxy-2-(methylsulfonyl)benzene | HCID 67092927 | 45% |
反応手順
1-Methanesulfonyl-3-methoxy benzene was dissolved in 90 mL glacial acetic acid. 100 mL water was added. A solution of bromine (4.79 g, 30 mmol) in 10 mL acetic acid was added dropwise at 10° C. The stirring was continued at rt for 15 h. The pH of the mixture was adjusted to pH 8 with aqueous NaOH solution, and extracted with EtOAc (3×200 mL) and dried over Na2SO4. The crude compound was purified by column chromatography (SilicaGel 230-400 mesh; 20% EtOAc in hexanes as an eluent) to give 1-bromo-2-methanesulfonyl-4-methoxy benzene (2.4 g, 45%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07846915B2 |
| 出典データセット | uspto-grants-2010_12 |
| ORD ID | ord-746692fdcb1e4ef4ba629fc6c100c760 |
| 出典メモ | uspto-grants-2010_12 |