関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanolamine | HCID 700 | — |
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 6-Chloro-2-methylpyrimidin-4-amine | HCID 286754 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-((6-Amino-2-methylpyrimidin-4-yl)amino)ethanol | HCID 69671185 | 40% |
反応手順
A mixture of 6-chloro-2-methylpyrimidin-4-ylamine (717 mg, 5.0 mmol) and ethanolamine (0.602 mL, 10.0 mmol) were heated at 250° C. in a microwave for 30 seconds. After cooling, the residue was dissolved in ethyl acetate, containing a small amount of methanol and was washed with brine. The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to afford the title compound as a white solid (334 mg, 40% yield). 1H NMR (400 MHz, DMSO-d6): δ 6.45 (br s, 1H), 5.98 (br s, 2H), 5.25 (s, 1H), 3.47 (t, J=6.0 Hz, 2H), 3.23-3.14 (m, 2H), 2.12 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09309240B2 |
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| 出典データセット | uspto-grants-2016_04 |
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| ORD ID | ord-6f4aad3310c7482bb8152eb6608ccce9 |
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| 出典メモ | uspto-grants-2016_04 |
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