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Sodium Carbonate → 5-Chloro-1-(3-thienylmethyl)pyrimidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-(Bromomethyl)thiophene | HCID 520703 | — |
| 反応物 | 5-Chloropyrimidin-2-ol hydrochloride | HCID 12648523 | — |
| 触媒 | Benzyltrimethylammonium chloride | HCID 5963 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 5-Chloro-1-(3-thienylmethyl)pyrimidin-2-one | HCID 20491759 | 34.2% |
反応手順
A mixture of 5-chloropyrimidin-2-one hydrochloride (502 mg), 3-bromomethylthiophene (1.069 g), anhydrous sodium carbonate (955 mg) and benzyltrimethylammonium chloride (12 mg) in dry N,N-dimethylformamide (15 ml) was stirred at room temperature. After 22 h the reaction mixture was diluted with water (120 ml) and the resulting precipitate was collected, washed with water and dried to give a pale yellow solid (233 mg). The solid was crystallised from ethanol to give white crystals of the title thiophene (184 mg), m.p. 194°-195° C., λmax 229 nm (ε 14,410), 233 nm (ε 3,080), λinf 246 nm (ε 5,210).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04399140 |
| 出典データセット | uspto-grants-1983_08 |
| ORD ID | ord-2b8a98689de64f6a9cfeb696e26be292 |
| 出典メモ | uspto-grants-1983_08 |