化工社化工社 化学情報印刷レポート · 研究参考用
Ethyl 2-formyl-3-(6-methyl-3-pyridyl)propionate → 5-((6-Methyl-3-pyridyl)methyl)-2-(nitroamino)-1H-pyrimidin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl 2-formyl-3-(6-methyl-3-pyridyl)propionate | HCID 3018359 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 反応物 | Nitroguanidine | HCID 86287517 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 5-((6-Methyl-3-pyridyl)methyl)-2-(nitroamino)-1H-pyrimidin-4-one | HCID 3018360 | 27.3% |
反応手順
A solution of ethyl 2-formyl-3-(6-methyl-3-pyridyl)propionate (1.55 g) in methanol (20 ml) was added to a solution of sodium methoxide (from 0.161 g sodium) in methanol (20 ml). Dried nitroguanidine (0.729 g) was added over 5 minutes and the mixture was stirred and boiled under reflux overnight and evaporated to dryness. The residue was dissolved in water (50 ml) and the solution was extracted with chloroform (2×25 ml, discarded) and acidified to pH 5 with acetic acid. The solid which precipitated out was filtered off and recrystallised from methanol-acetic acid to give 2-nitroamino-5-(6-methyl-3-pyridylmethyl)-4-pyrimidone (0.5 g) m.p. 215°-216° (decomp.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04234588 |
| 出典データセット | uspto-grants-1980_11 |
| ORD ID | ord-46642644a8ee4d13ad3d1e29c7f3f7da |
| 出典メモ | uspto-grants-1980_11 |