化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 178498045、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | N-Acetylimidazolidinone | HCID 79350 | — |
| 反応物 | Methyl 4-amino-3,5-dichlorobenzoate | HCID 604808 | — |
| 溶媒 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | HCID 178498045 | HCID 178498045 | 75.2% |
反応手順
Methyl-4-amino-3,5-dichlorobenzoate (16.8 g, 31 mmole), 1-acetyl-2-imidazolidone (4.3 g, 33.5 mmole) in phosphoryl chloride (44 ml) were stirred at 50° C. for 3 days. After cooling the phosphoryl chloride was evaporated to give an oily residue. Iced water was added to the residue which was then basified with aqueous sodium hydroxide. The mixture was extracted with methylene chloride which was then washed with water, dried (magnesium sulphate) and evaporated to give a creamy solid. This solid was recrystallised from toluene to give the title compound (7.7 g) mp 188°-189° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04505926 |
| 出典データセット | uspto-grants-1985_03 |
| ORD ID | ord-026a6d3952fa4328a8677a98144acf0c |
| 出典メモ | uspto-grants-1985_03 |