関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 1-Fluoroethan-1-ol | HCID 19359348 | — |
| 反応物 | N-[6-chloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide | HCID 53744388 | — |
| 生成物 | HCID 54459196 | HCID 54459196 | — |
反応手順
To a solution of 258 mg of fluoroethanol in 20 ml of dimethylformamide was added 194 mg of sodium hydride (60%) with ice cooling followed by stirring for 30 minutes. To this reaction solution was added 400 mg of N-[6-chloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide with stirring under ice cooling followed by stirring for 30 minutes. The reaction mixture was stirred at room temperature for two hours and poured into a mixture of 1N hydrochloric acid and ice. This solution was extracted with chloroform and the chloroform layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated in vacuo and the resulting residue was purified by a silica gel column chromatography (chloroform-methanol=40:1). The resulting amorphous substance was crystallized in ether and collected by filtration to give 240 mg of N-[6-(2-fluoroethoxy)-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06083955 |
|---|
| 出典データセット | uspto-grants-2000_07 |
|---|
| ORD ID | ord-bfa7725063f34ec0842ee2fd7289006b |
|---|
| 出典メモ | uspto-grants-2000_07 |
|---|