関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl formate | HCID 8025 | — |
| 反応物 | 2-Phenylmalonamide | HCID 2747536 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | HCID 178518202 | HCID 178518202 | 69.1% |
反応手順
Sodium metal (0.92 g, 40 mmol) was dissolved by stirring in ethanol (30 mL) at room temperature under argon over 40 min. To the resulting solution at room temperature was added 2-phenylmalonamide (3.56 g, 20 mmol) and ethyl formate (1.9 mL, 24 mmol). The resulting suspension was heated at 50° C. under argon 16 h. After cooling the reaction mixture to room temperature, water (100 mL) was added and the mixture was stirred for 1 h. Solid was removed by filtration. The filtrate was acidified to pH˜4 with 1 M aqueous HCl. The resulting precipitate was collected by filtration and further washed with water (20 mL×2), then Et2O (10 mL×2). After drying under vacuum for 3 h, the title compound (2.6 g) was obtained as a light yellow solid. HPLC/MS: retention time=0.76 min, [M+H]+=189.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07452892B2 |
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| 出典データセット | uspto-grants-2008_11 |
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| ORD ID | ord-688288197ef7443e83e0b009843faba2 |
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| 出典メモ | uspto-grants-2008_11 |
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