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Triethylamine → 2-[(2-chloro-3-nitrophenyl)methylsulfanyl]-6-methyl-1H-pyrimidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(Bromomethyl)-2-chloro-3-nitrobenzene | HCID 18363045 | — |
| 反応物 | HCID 178429541 | HCID 178429541 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-[(2-chloro-3-nitrophenyl)methylsulfanyl]-6-methyl-1H-pyrimidin-4-one | HCID 178429439 | 64% |
反応手順
6-methyl-2-sulfanylpyrimidin-4-ol (200 mg, 1.4 mmol) was dissolved in absolute ethanol (15 mL), then triethylamine (230 μL, 1.7 mmol) and 1-(bromomethyl)-2-chloro-3-nitrobenzene (350 mg, 1.4 mmol) were added. The mixture was stirred overnight at room temperature. The solid was filtered, washed with methanol, and then dried in vacuo to afford 2-{[(2-chloro-3-nitrophenyl)methyl]sulfanyl}-6-methylpyrimidin-4-ol as white solid (277 mg, 64% yield); 1H NMR (400 MHz, DMSO-d6): δ 2.23 (s, 3H), 4.56 (s, 2H), 6.00 (bs, 1H), 7.56 (t, J=7.9 Hz, 1H), 7.95 (d, J=8.2 Hz, 2H); LRMS (ES+) m/z 312 (100%, M+1), 314 (45%, M+3).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09040538B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-cfceb032ac2344e1a95b94f1266a0035 |
| 出典メモ | uspto-grants-2015_05 |