関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-(4-Hydroxy-3-Methoxyphenyl)Prop-2-Enoic Acid | HCID 709 | — |
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 11185931 | HCID 11185931 | 93% |
反応手順
3-methoxy-4-hydroxy-cinnamic acid (8 g, 41.2 mmol) and imidazole (8.4 g, 123.6 mmol) were charged in a 500 mL round-bottom flask and dissolved in 30 mL of dimethylformamide. Tert-butyldimethylsilyl chloride (13.04 g, 86.5 mmol) was added thereto at 0° C., followed by stirring for 30 minutes. The reaction liquid was concentrated by distillation under reduced pressure and dichloromethane (200 mL) was added thereto, followed by washing with water. The organic layer was dried over anhydrous magnesium sulfate, concentrated and dissolved in tetrahydrofuran (180 mL)/methanol (500 mL), and a 0.00035M potassium carbonate aqueous solution (175 mL) was added thereto, followed by stirring for 1 hour. After being concentrated by distillation under reduced pressure, the resulting solid was filtered, washed with water, and dried under vacuum to afford the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08637674B2 |
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| 出典データセット | uspto-grants-2014_01 |
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| ORD ID | ord-a791b323335748f0a6cc4abc4ce47047 |
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| 出典メモ | uspto-grants-2014_01 |
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