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Lithium hydroxide, monohydrate → 3-Iodo-5-(5-methyl-pyridin-2-yl)-benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium hydroxide, monohydrate | HCID 168937 | — |
| 反応物 | 3-Iodo-5-(5-methyl-pyridin-2-yl)-benzoic acid methyl ester | HCID 59432579 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Iodo-5-(5-methyl-pyridin-2-yl)-benzoic acid | HCID 59599701 | 93% |
反応手順
A solution of LiOH hydrate (82 mg, 1.94 mmol) in H2O (7 mL) was added dropwise to a suspension of 3-iodo-5-(5-methyl-pyridin-2-yl)-benzoic acid methyl ester (526 mg, 1.49 mmol) in THF (4 mL) at 0° C. The reaction mixture was allowed to warm to room temperature and was stirred until the reaction solution turned into clear. Solvent was removed under vacuum and the resulting aqueous solution was acidified by 10% HCl to pH=6-7. The resulting precipitate was collected and dried to afford 3-iodo-5-(5-methyl-pyridin-2-yl)-benzoic acid (470 mg, 93%). MS (M+H)=340.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08440708B2 |
| 出典データセット | uspto-grants-2013_05 |
| ORD ID | ord-20b88bf15c3147499984d9a22868d102 |
| 出典メモ | uspto-grants-2013_05 |