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Hydrochloric Acid → 4-(4-Bromo-2,5-dichloro-phenoxy)-6-methyl-nicotinic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | 4-(4-Bromo-2,5-dichloro-phenoxy)-6-methyl-nicotinic acid methyl ester | HCID 67320549 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(4-Bromo-2,5-dichloro-phenoxy)-6-methyl-nicotinic acid | HCID 67319480 | 100% |
反応手順
To a solution of 185 mg (0.473 mmol) 4-(4-bromo-2,5-dichloro-phenoxy)-6-methyl-nicotinic acid methyl ester in 3 mL dioxane was added 3 mL water and 30 mg (0.710 mmol) lithium hydroxide monohydrate. The reaction mixture was stirred for 4 hours at room temperature, poured on 30 mL 1M aqueous hydrochloric acid and 30 mL dichloromethane and the layers were separated. The aqueous layer was extracted with 30 mL dichloromethane and the combined organic layers were washed with 30 mL brine, dried over magnesium sulfate, filtered and concentrated under vacuum to afford 178 mg (100%) of the title compound as a colorless solid. MS (ESI): m/z=377.912 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08729091B2 |
| 出典データセット | uspto-grants-2014_05 |
| ORD ID | ord-111e8dd2f19d443c855c7bb843f91553 |
| 出典メモ | uspto-grants-2014_05 |