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Triethylamine → 1-(3-Methylphenylthio)methyl-5-fluoropyrimidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Fluoropyrimidin-2-one | HCID 101498 | — |
| 反応物 | Potassium Bromide | HCID 253877 | — |
| 反応物 | 3-Methylphenyl chloromethyl sulfide | HCID 12840894 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(3-Methylphenylthio)methyl-5-fluoropyrimidin-2-one | HCID 15650500 | — |
反応手順
3-(Chloromethylthio)toluene (6.5 mmol) was added to a solution of 5-fluoropyrimidin-2-one (6.5 mmol) and triethylamine (6.5 mmol) in dichloromethane (75 ml) and the resultant mixture heated under reflux for 2 days. The solvent was then distilled off, the residue triturated with water and the residual material extracted with CCl4. Evaporation of the extracts and crystallisation of the residue from ethyl acetate gave the pure product; 0.40 g (25%), m.p. 124° C. (Found: C57.42; H4.63. Calc. for C12H11FN2OS: C57.59; H4.43) 1H NMR (DMSO d6); δ 2.28 (Me), 5.17(CH2), 7.2 (Ph), 8.05 (H-4), 8.70 (H-6). IR (KBr): 1670 cm-1 (CO), MS [70 eV, m/z (% rel. int.)]: 250 (8,M), 137(11), 136(36), 135(10), 128(7), 127(100), 100(34), 91(9).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04705791 |
| 出典データセット | uspto-grants-1987_11 |
| ORD ID | ord-be950a6fa23d444c879577fb33e2a1e5 |
| 出典メモ | uspto-grants-1987_11 |