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Bromine → 4-Bromo-2-(trifluoromethoxy)phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | 2-(Trifluoromethoxy)phenol | HCID 2777299 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Bromo-2-(trifluoromethoxy)phenol | HCID 11780151 | — |
反応手順
1.55 mL (30.3 mmol) bromine in 50 mL DCM is added dropwise to a solution of 5.0 g (28.1 mmol) 2-trifluoromethoxy-phenol in 70 mL DCM at −78° C. The reaction solution is heated to RT and stirred for a further 48 h. Then 70 mL Na2SO3 solution are added and the mixture is stirred until the orange colour has disappeared. The solution is diluted with DCM, the organic phase is washed with NaCl solution, dried over MgSO4 and the solvent is eliminated i.vac. The purification is carried out by column chromatography on silica gel (gradient: PE to PE:EtOAc 4:1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07452911B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-bcf3a28d542a4787bc28760aa1133a9a |
| 出典メモ | uspto-grants-2008_11 |