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Benzamidine → 6-Oxo-4-(4-phenoxyphenyl)-2-phenyl-1,6-dihydropyrimidine-5-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzamidine | HCID 2332 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | (E)-ethyl 2-cyano-3-(4-phenoxyphenyl)acrylate | HCID 86665688 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 6-Oxo-4-(4-phenoxyphenyl)-2-phenyl-1,6-dihydropyrimidine-5-carbonitrile | HCID 136372349 | — |
反応手順
A mixture of (E)-ethyl 2-cyano-3-(4-phenoxyphenyl)acrylate (100 mg, 0.341 mmol) and benzamidine (45.1 mg, 0.375 mmol) in methanol (1 mL) was stirred at room temperature for 15 h while opening to the air. The mixture was treated with ethyl acetate (30 mL), washed with water (5 mL), brine (5 mL), dried (MgSO4) and concentrated to give crude 6-oxo-4-(4-phenoxyphenyl)-2-phenyl-1,6-dihydropyrimidine-5-carbonitrile as tan solid. The crude material was taken to next reaction without purification. MS (ES+) m/z: 366 (M+H); LC retention time: 4.525 min (analytical HPLC Method B).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846673B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-9b38a98df425408583cd019796b1d46e |
| 出典メモ | uspto-grants-2014_09 |