関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Fluorophenol | HCID 9732 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | tert-Butyl N-(2-((methylsulfonyl)oxy)ethyl)carbamate | HCID 22605302 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (2-(4-Fluorophenoxy)-ethyl)-carbamic acid tert-butyl ester | HCID 23134036 | 57.4% |
反応手順
Next, to a solution of 4-fluorophenol (0.47 g, 4.18 mmol) in DMF (10 mL) was added cesium carbonate (2.72 g, 8.36 mmol) at room temperature. The mixture was stirred at ambient temperature for 15 minutes, then methanesulfonic acid 2-(tert-butoxycarbonylamino)ethyl ester (1.00 g, 4.18 mmol) was added. The reaction mixture was stirred at 100° C. for 16 hours. Water was added and the mixture was concentrated in vacuo. Product mixture was dissolved in ethyl acetate and was washed with water, then with brine. The organic layer was dried over Na2SO4, and the solvent was removed under reduced pressure. The residue was purified by column chromatography (ethyl acetate:hexane=7:1 to 4:1), and obtained [2-(4-fluorophenoxy)ethyl]carbamic acid tert-butyl ester as yellow oil (0.61 g, 57.4% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07423175B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-6ea6e05ed63f45a6a9ae7d06ee7857cb |
|---|
| 出典メモ | uspto-grants-2008_09 |
|---|