関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Dimethoxybenzoic Acid | HCID 15109 | — |
| 反応物 | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Dimethyl Carbonate | HCID 12021 | — |
| 生成物 | Benzoic acid, 2,6-dimethoxy-, methyl ester | HCID 137419 | — |
反応手順
1,8-diazabicyclo[5.4.0]undec-7-ene (DBU), (836 mg, 5.49 mmol), was added to a mixture of 2,6-dimethoxybenzoic acid (1), (1.0 g, 5.49 mmol), in dimethyl carbonate (DMC) (10 mL) and the resulting mixture was heated to reflux at 90° C. for 4 hours. The reaction mixture was cooled to 25° C. and diluted with EtOAc (30 mL) and water (30 mL). The organic layer was separated and washed in sequence with 10 mL of water, 2 M HCl (2×30 mL), saturated aqueous NaHCO3 (2×30 mL) and water (2×25 mL). The organic layer was dried over Na2SO4, filtered and concentrated under vacuum to give methyl 2,6-dimethoxybenzoate (2) as a white solid. The yield of the 2,6-dimethoxybenzoate as determined by HPLC was 97-98% conversion.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06515167B1 |
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| 出典データセット | uspto-grants-2003_02 |
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| ORD ID | ord-107e392ba5f74beaa591bfe07c008edd |
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| 出典メモ | uspto-grants-2003_02 |
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