関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | Iodine chloride | HCID 24640 | — |
| 反応物 | Methyl 4-amino-3-chloro-6-(2,5-difluoro-4-(trimethylsilyl)phenyl)-5-fluoropicolinate | HCID 90409474 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Methyl 4-amino-3-chloro-6-(2,5-difluoro-4-iodophenyl)-5-fluoropicolinate | HCID 90409448 | 74.4% |
反応手順
To a solution of methyl 4-amino-3-chloro-6-(2,5-difluoro-4-(trimethylsilyl)phenyl)-5-fluoropicolinate (0.280 g, 0.720 mmol) in CH2Cl2 (2.88 mL) at 20° C. was added iodine monochloride (0.144 mL, 2.880 mmol). The reaction mixture was stirred at 20° C. overnight. The mixture was then poured into a 10% aqueous solution of Na2SO3, extracted with EtOAc (3×), dried over Na2SO4, filtered and concentrated. The residue was purified by flash column chromatography (SiO2, hexanes/EtOAc gradient) to afford the title compound as a white solid (0.237 g, 0.536 mmol, 74.4%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09113629B2 |
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| 出典データセット | uspto-grants-2015_08 |
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| ORD ID | ord-25645352d02d493fb79f4cae7e88543c |
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| 出典メモ | uspto-grants-2015_08 |
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