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Sodium Hydroxide → 5-Chloro-4-iodo-2-methoxybenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Methyl 5-chloro-4-iodo-2-methoxybenzoate | HCID 69314795 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-Chloro-4-iodo-2-methoxybenzoic acid | HCID 16791858 | 91.9% |
反応手順
A mixture of 5-chloro-4-iodo-2-methoxy benzoic acid methyl ester of Step B (3.00 g, 9.19 mmol) and sodium hydroxide (1.10 g, 27.6 mmol) in methanol (92 mL) was refluxed for 12 hours. The reaction was cooled to room temperature and the solvent evaporated. The residue was dissolved in 1 N sodium hydroxide (75 mL), the solution washed with diethyl ether and the organic washings discarded. The aqueous phase was acidified with 2 N HCl and extracted with diethyl ether. The combined extracts were dried over anhydrous sodium sulfate, filtered and concentrated to afford the title carboxylic acid (2.64 g) as orange crystals, m.p. 150-151° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06903087B2 |
| 出典データセット | uspto-grants-2005_06 |
| ORD ID | ord-49103f9fcb314fbf85fa4ff56901cce8 |
| 出典メモ | uspto-grants-2005_06 |