関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | N-Cyclohexylaniline | HCID 74567 | — |
| 反応物 | 5-Bromo-2,4-dichloropyrimidine | HCID 289973 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 生成物 | (5-Bromo-2-chloro-pyrimidin-4-yl)-cyclohexyl-phenyl-amine | HCID 58299589 | 24% |
反応手順
5-Bromo-2,4-dichloro-pyrimidine (2.17 ml, 17.14 mmol) and cyclohexyl-phenyl-amine (2.0 g, 11.43 mmol) were dissolved in N-methylpyrrolidone (NMP) (25 ml), and this reaction was heated to 120° C. for 24 hours. The reaction was cooled to room temperature and diluted with ethyl acetate, washed with water and brine. The organic phase was dried using sodium sulfate and concentrated. Purification by flash chromatography (ethyl acetate/hexane) gave compound 37 as a yellow solid (855 mg, 24%). 1H NMR (500 MHz, DMSO-d6) δ ppm 8.27 (1 H, s), 7.41 (3 H, m), 7.21 (2 H, m), 4.62 (1 H, m), 1.93 (2 H, d, J=10 Hz), 1.75 (2 H, d, J=10 Hz), 1.58 (1 H, d, J=10 Hz), 1.34 (2 H, m), 1.15 (2 H, m), 0.91 (1 H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841312B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-6e09e02edeb2407fa29c35bb3c7b1f63 |
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| 出典メモ | uspto-grants-2014_09 |
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