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3,5-Dichloro-1-fluoropyridinium triflate → Methyl 5-fluoro-4-hydroxy-2-methoxybenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,5-Dichloro-1-fluoropyridinium triflate | HCID 2724578 | — |
| 反応物 | Methyl 4-hydroxy-2-methoxybenzoate | HCID 12532676 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 5-fluoro-4-hydroxy-2-methoxybenzoate | HCID 18914108 | — |
反応手順
To a stirred solution of the methyl 4-hydroxy-2-methoxybenzoate (1 g, 5 mmol, from Step 3) in CH2Cl2 (20 mL) was added 3,5-dichloro-1-fluoropyridinium triflate (2.25 g, 6 mmol). The solution was refluxed for 48 h and then cooled to ambient temperature and stripped down under reduced pressure. The crude oil was purified by pressurized silica gel column chromatography using 99:1 CH2Cl2 :MeOH. Evaporation of the CH2Cl2 :MeOH mixture gave the desired methyl 5-fluoro-4-hydroxy-2-methoxybenzoate as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726172 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-48df0370b6c1448ea65c1fd6355a24c2 |
| 出典メモ | uspto-grants-1998_03 |