化工社化工社 化学情報印刷レポート · 研究参考用
Cyanoacetic acid → 1-(2-Cyanoacetyl)-3-(2-fluoro-4-iodophenyl)-urea
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyanoacetic acid | HCID 9740 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | Propan-2-ol--water (1/1) | HCID 21889133 | — |
| 反応物 | (2-Fluoro-4-iodophenyl)-urea | HCID 59717008 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(2-Cyanoacetyl)-3-(2-fluoro-4-iodophenyl)-urea | HCID 59717317 | — |
反応手順
To a mixture of (2-fluoro-4-iodophenyl)-urea 78 (21.7 g) and cyanoacetic acid 73 (7.88 g) in N,N-dimethylformamide (108 ml) was added, and methanesulfonyl chloride (7.17 ml) was added dropwise with stirring at room temperature. The mixture was stirred at room temperature for 2 hrs, and water-isopropyl alcohol [1:2 (volume ratio), 210 ml] was added dropwise. The mixture was stirred at room temperature for 1 hr. The precipitated crystals were collected by filtration and washed with water to give 1-(2-cyanoacetyl)-3-(2-fluoro-4-iodophenyl)-urea 79 (wet crystals), which was used for the next reaction in the form of wet crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835443B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-1a932bf29f6e486bba32a6e38f9030a0 |
| 出典メモ | uspto-grants-2014_09 |