関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | HCID 86682905 | HCID 86682905 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Fluoro-3,6-dimethoxybenzoic acid | HCID 84775696 | 98.2% |
反応手順
To a mixture of ethyl 2-fluoro-3,6-dimethoxybenzoate (8.1 g, 35.5 mmol) in methanol (150 mL) and water (50 mL), lithium hydroxide (7.5 g, 178 mmol) was added. The resulting mixture was heated at 80° C. for 5 h. The reaction mixture was concentrated to remove methanol, acidified with 2 M HCl until pH 4, and extracted with dichloromethane (4×200 mL). The combined organic layers were dried (Na2SO4) and concentrated under reduced pressure to give the title compound (6.98 g). 1H NMR (DMSO-d6): δ 13.39 (br s, 1H), 7.19 (t, 1H), 6.82 (dd, 1H), 3.79 (s, 3H), 3.75 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09078871B2 |
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| 出典データセット | uspto-grants-2015_07 |
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| ORD ID | ord-1e9a8b5b95584842a611b16d8b3c8e59 |
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| 出典メモ | uspto-grants-2015_07 |
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