関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanimidamide, N,N-diphenyl- | HCID 78296 | — |
| 反応物 | 3-(3-Chlorophenyl)-3-oxopropanenitrile | HCID 140855 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(3-Chlorobenzoyl)-3-phenylaminoacrylonitrile | HCID 67024226 | 75.3% |
反応手順
A solution of 3-chlorobenzoylacetonitrile (476 mg, 2.66 mmol, 1.0 eq) and diphenylformamidine (522 mg, 2.66 mmol, 1.0 eq) in 25 mL of toluene was stirred at room temperature for 2 h then heated to 100° C. overnight. The solution was cooled and diluted with hexanes. The resulting solid was filtered and dried to provide the desired product (566 mg, 75%). HPLC (4 minute 10-95 gradient) tR 2.97 min; MS m/z 283.2 [M+H]+; 1H NMR (CDCl3), δ 8.06 (d, J=13.2 Hz, 1 H), 7.85 (m, 2 H), 7.46 (m, 4 H), 7.27 (m, 4 H) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08242117B2 |
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| 出典データセット | uspto-grants-2012_08 |
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| ORD ID | ord-6176add4139a43dd95444b42f78f9396 |
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| 出典メモ | uspto-grants-2012_08 |
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