関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 反応物 | 6-Chloro-n4-(4-methylphenyl)pyrimidine-2,4-diamine | HCID 238748 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N4,N4-dimethyl-N6-(4-methylphenyl)-2,4,6-pyrimidinetriamine | HCID 68563652 | 40% |
反応手順
A mixture of 6-chloro-N4-(4-methylphenyl)-2,4-pyrimidinediamine (1.5 g, 6.4 mmol), and N,N-dimethylamine hydrochloride (0.56 g, 7 mmol) and triethylamine (1.4 g, 14 mmol) in DMF (2 mL), was heated at 170° C. for 16 h. The product was filtered out and the organic layer was treated with saturated NaHCO3 (50 mL) and extracted with EtOAC (3×50 mL). The organic layer washed with brine (2×100 mL), dried over Na2SO4, filtered, and concentrated in vacuo. The crude product was purified by chromatography on silica using hexane/EtOAc (1:3), giving the desired product (0.6 g, 40%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07465750B2 |
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| 出典データセット | uspto-grants-2008_12 |
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| ORD ID | ord-16b85103ebd746afb7df50311114ad60 |
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| 出典メモ | uspto-grants-2008_12 |
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