関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Aminocyclopropane-1-carboxylic acid | HCID 535 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 生成物 | Ethyl 1-aminocyclopropane-1-carboxylate hydrochloride | HCID 386203 | 100% |
反応手順
A suspension of 1-aminocyclopropanecarboxylic acid (5.8 g, 57.4 mmol) in 300 mL of ethanol was cooled to 0° C., thionyl chloride (20.5 g, 172.7 mmol) was added drop-wise over 30 minutes. Then the cold bath was removed and the reaction mixture was heated at reflux for 2 hours, then the mixture was stirred at room temperature for 16 hours. The solvent was evaporated at 40° C. under reduced pressure to give ethyl 1-aminocyclopropanecarboxylate hydrochloride (9.53 g, 100%) as a solid. It was used directly in the next step without further purification. MS: (M+H)+=130.2; 1H NMR (300 MHz, DMSO): δ 9.04 (brs, 3H), 4.14 (q, 2H, J=6.9 Hz), 1.45 (d, 2H, J=3.3 Hz), 1.37 (d, 2H, J=3.2 Hz), 1.19 (t, 3H, J=6.9 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08658646B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-dd1342184d5548d2935f6b562c20a59e |
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| 出典メモ | uspto-grants-2014_02 |
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