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Glutaric anhydride → 4-[(4-Ethynylphenyl)carbamoyl]butanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Glutaric anhydride | HCID 7940 | — |
| 反応物 | 4-Ethynylaniline | HCID 3760025 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-[(4-Ethynylphenyl)carbamoyl]butanoic acid | HCID 24826477 | 96% |
反応手順
Glutaric anhydride (540 mg, 4.70 mmol) was dissolved in anhydrous dichloromethane (7 mL) and followed with the addition of p-aminophenyl-acetylene (500 mg, 4.27 mmol). The mixture was allowed to stir at room temperature for 6 hours before the solvent was evaporated under reduced pressure to provide 900 mg of a yellow white product 24 (96%); mp 135-140° C.; 1H NMR (DMSO-d6, 300 MHz) δ 1.77 (p, J=8.21 Hz, 2H), 2.25 (t, J=9.30 Hz, 2H), 2.34 (t, J=6.56 Hz, 2H), 4.05 (s, 1H), 7.38 (d, J=8.52 Hz, 2H), 7.59 (d, J=7.91 Hz, 2H) 9.90 (s, 1H); HRMS m/e calculated for (M+H)+: C13H13NO3 231.0895; found 231.0895.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745229B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-ff5b7f31a9314cb5b8450f6baebb601a |
| 出典メモ | uspto-grants-2010_06 |