関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Thiophenecarboxylic acid | HCID 10700 | — |
| 反応物 | 3-Methoxyphenethylamine | HCID 74866 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 反応物 | 1-(3-Diethylaminopropyl)-3-ethylcarbodiimide hydrochloride | HCID 9964512 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 47222443 | HCID 47222443 | 107.6% |
反応手順
A mixture of 3-methoxyphenethylamine (1.000 g, 6.61 mmol), 2-thiophenecarboxylic acid (0.847 g, 6.61 mmol), 1-hydroxybenzotriazole hydrate (1.340 g, 9.92 mmol), and 1-(3-diethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.330 g, 6.94 mmol) in anhydrous CH2Cl2 (20 ml) was stirred at 0° C. under N2 for 1 hr, then warmed to rt and stirred at rt for 18 hr. The reaction mixture was washed with 1M NaOH (10 ml) followed by 1M HCl (10 ml), dried over MgSO4, and concentrated in vacuo to give 1.859 g of yellow oil. Purification by flash chromatography, eluting with hexane:EtOAc (7:3) gave 1.637 g (95% yield) of yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06608203B2 |
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| 出典データセット | uspto-grants-2003_08 |
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| ORD ID | ord-383e5819d9164389b3de5122ca6e2c14 |
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| 出典メモ | uspto-grants-2003_08 |
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