化工社化工社 化学情報印刷レポート · 研究参考用
Water → Methyl-phenyl-carbamic Acid 5-(3,4-dichloro-phenoxy)-pyrimidin-2-yl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | Carbamic chloride, N-methyl-N-phenyl- | HCID 77969 | — |
| 反応物 | HCID 178517841 | HCID 178517841 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Methyl-phenyl-carbamic Acid 5-(3,4-dichloro-phenoxy)-pyrimidin-2-yl Ester | HCID 69518926 | 65.3% |
反応手順
A solution of 5-(3,4-dichloro-phenoxy)-pyrimidin-2-ol (0.51 g, 2.00 mmol), N-methyl-N-phenylcarbamoyl chloride (0.34 g, 2.00 mmol) and 1,4-diazabicyclo[2.2.2]octane (0.22 g, 2.00 mmol) in dimethylformamide (15 ml) was stirred at room temperature for 1 hour. Water was added and the precipitates were collected by suction. The solids were dissolved in dichloromethane and the solution was dried over sodium sulphate, filtered and evaporated in vacuo. The residue was crystallised from ethyl acetate:heptane yielding the title compound (0.51 g, 65% yield) as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07279470B2 |
| 出典データセット | uspto-grants-2007_10 |
| ORD ID | ord-d42fde9100064f73b3a6c0b00d59fff9 |
| 出典メモ | uspto-grants-2007_10 |