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Sodium Hydroxide → 1-Methyl 2,6-dichloro-1,4-benzenedicarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Dimethyl 2,6-dichloroterephthalate | HCID 7730227 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Methyl 2,6-dichloro-1,4-benzenedicarboxylate | HCID 18673016 | 41% |
反応手順
To a solution of dimethyl 2,6-dichloroterephthalate (186 g, 707 mmol) in THF (600 mL) at room temperature was added a solution of sodium hydroxide (29.7 g, 742 mmol) in water (600 mL). The reaction mixture was stirred at room temperature for 48 hours and concentrated under reduce pressure to a volume of 600 mL. The residue was diluted with water (400 mL), cooled to 0° C. and acidified with 1 N HCl (800 mL). The resulting precipitate was collected by filtration and dried in vacuo to give 3,5-dichloro-4-(methoxycarbonyl)benzoic acid (72 g, yield: 41%) as a white solid: 1H NMR (400 MHz, DMSO-d6) δ 3.90 (s, 3H), 7.92 (s, 2H). LCMS (ESI) m/z: 249.0 [M+H+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08486950B2 |
| 出典データセット | uspto-grants-2013_07 |
| ORD ID | ord-dc4e716fcd2045819e928afaa7badd4e |
| 出典メモ | uspto-grants-2013_07 |