関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-chloro-N-methyl-5-nitropyrimidin-4-amine | HCID 7147232 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Chloro-N4-methylpyrimidine-4,5-diamine | HCID 7147172 | 69.4% |
反応手順
To a stirred solution of 2-chloro-N-methyl-5-nitropyrimidin-4-amine (1.9 g, 10 mmol) in acetic acid (30 mL) was added iron powder (4 g, 71 mmol), and the suspension mixture was heated to 60° C. for 16 hours. The solvent was removed under reduced pressure, and the residue was diluted by brine and ethyl acetate. The solid was filtered off, and the filtrate was extracted with ethyl acetate (50 mL*12). The organic layers were separated, combined, dried over sodium sulfate, filtered and concentrated to give the title compound (1.1 g, 69%). MS (ES+) C5H7ClN4 requires: 159, 161. found: 160, 162 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09340514B2 |
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| 出典データセット | uspto-grants-2016_05 |
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| ORD ID | ord-56951a43107a4a83be3043c748893928 |
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| 出典メモ | uspto-grants-2016_05 |
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