関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Glycinamide hydrochloride | HCID 2723639 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Ethyl 3-(2,5-dimethoxyphenyl)-3-oxopropanoate | HCID 12297472 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (Z)-Ethyl 3-((2-amino-2-oxoethyl)amino)-3-(2,5-dimethoxyphenyl)acrylate | HCID 86684673 | 106.9% |
反応手順
A 5-L reaction vessel was charged with methanol (3.3 L), sodium methoxide (102.4 g, 1.8 moles), and glycinamide hydrochloride (202 g, 1.8 moles). The mixture was heated at 65° C. for 1 hour before cooling to 50° C. and adding acetic acid (514.25 mmoles, 30.88 g, 29.47 mL) and ethyl 3-(2,5-dimethoxyphenyl)-3-oxopropanoate (300 g, 1.03 mole). After heating at reflux for 16 hours, the reaction mixture was stirred as it was cooled to 10° C. After 30 min the resulting solid was collected by vacuum filtration, pulling dry to form a cake that was dried in a vacuum oven (20 mm Hg, 65° C.) for 14 hours to afford the title compound (339.4 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08841314B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-766db1b16ef944a4be88488959b1a3b8 |
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| 出典メモ | uspto-grants-2014_09 |
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