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Diethylcarbamoyl chloride → n,n-Diethyl-(3-morpholin-4-yl-phenoxy)carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethylcarbamoyl chloride | HCID 6916 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Morpholinophenol | HCID 141343 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | n,n-Diethyl-(3-morpholin-4-yl-phenoxy)carboxamide | HCID 9878759 | — |
反応手順
To a stirred mixture of 3-morpholinylphenol (0.34 g; 1.9 mmol) and powdered K2CO3 (0.576 g; 4.2 mmol) in dry acetonitrile (10 mL) was added diethyl carbamylchloride (0.26 mL; 2.0 mmol) via syringe at room temperature under nitrogen atmosphere. The resulting mixture was heated to reflux for 24 hours, then allowed to cool to room temperature. The reaction was diluted with EtOAc (60 mL), washed with water (2×20 mL) and brine, then dried (MgSO4), filtered, and concentrated in vacuo. The residue was purified via radial chromatography (4 mm chromatotron plate with 2:1 hexanes/EtOAc) to provide the carbamate as a clear, colorless oil (0.39 g; 74%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07179912B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-b76ca35572524a9080b7fb265fe43dee |
| 出典メモ | uspto-grants-2007_02 |