化工社化工社 化学情報印刷レポート · 研究参考用
Methylurea → 1-Methylimidazolidine-2,4,5-trione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methylurea | HCID 11719 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Methylimidazolidine-2,4,5-trione | HCID 123196 | 94.3% |
反応手順
To an ice-cold solution of 1-methylurea (200 mg, 2.70 mmol) in dry tetrahydrofuran (6 mL) was added oxalyl chloride (0.26 mL, 2.97 mmol) dropwise, under a nitrogen atmosphere. The reaction mixture was stirred at 0-5° for 2 h and then allowed to warm to room temperature for 1 h before being diluted with water. The product was extracted with ethyl acetate, and the extracts were washed with water, dried and evaporated to give the product as an off-white solid (326 mg, 94%), mp 146-149° C. (lit. 145-148° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835629B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-5270f0fd388c4422b4413078322e13df |
| 出典メモ | uspto-grants-2014_09 |