関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Isocyanate | HCID 105034 | — |
| 反応物 | (3R)-3-amino-3-phenylpropanoic acid | HCID 686703 | — |
| 生成物 | beta-[[[[4-Cyanophenyl]butyl]amino]carbonyl]aminobenzenepropanoic acid | HCID 54501418 | — |
反応手順
A solution of the isocyanate (6) (4.74 mmol), triethylamine (0.479 g, 4.74 mmol), β-phenylalanine (1.17 g, 7.11 mmol), and anhydrous DMF (10 mL) was warmed to 120° C. for 20 hours. After cooling to 23° C., the reaction mixture was concentrated on the rotovap, diluted with ethyl acetate (400 mL), washed with KHSO4 (1N, 2×100 mL), washed with brine (1×100 mL), and dried (Na2SO4). After concentration in vacuo, the urea was purified by flash chromatography (step gradient ethyl acetate with 1% acetic acid to ethyl acetate with 10% methanol and 1% acetic acid) to afford 1.49 g (86%) of(7).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05344837 |
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| 出典データセット | uspto-grants-1994_09 |
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| ORD ID | ord-c7d9ca83b83444cd9414f53c09849282 |
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| 出典メモ | uspto-grants-1994_09 |
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