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Chloroacetaldehyde → HCID 18001294、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroacetaldehyde | HCID 33 | — |
| 反応物 | 2-Amino-4-chloropyrimidine | HCID 223332 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 18001294 | HCID 18001294 | 67% |
反応手順
2-Amino-4-chloropyrimidine (1.00 g, 7.72 mmol) and sodium methoxide (1.25 g, 23.2 mmol) were suspended in methanol (20 ml) and heated under reflux for 2 h then cooled to ambient temperature. Chloroacetaldehyde (2.4 ml of a 45% w/w solution in water, 15.44 mmol) was added and the mixture heated under reflux for 22 h, allowed to cool to ambient temperature then pre-adsorbed directly onto silica. Purification by chromatography on silica gel eluting with dichloromethane (containing 1% conc. ammonia) on a gradient of methanol (1-4%) gave 7-methoxyimidazo[1,2-a]pyrimidine (0.77 g, 67%) as a white crystalline solid: δH (400 MHz, CDCl3) 4.04 (3H, s), 6.41 (1H, d, J 7), 7.31 (1H, d, J 1), 7.50 (1H, d, J 1), 8.17 (1H, d, J 7).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06642229B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-8e1ea295441a4334beabc5a39142bb53 |
| 出典メモ | uspto-grants-2003_11 |