関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexamethyldisilazane | HCID 13838 | — |
| 反応物 | Ammonium Sulfate | HCID 6097028 | — |
| 反応物 | 2-Acetylamino-3-cyclopropylamino-but-2-enoic acid ethyl ester | HCID 69290800 | — |
| 生成物 | Ethyl 1-cyclopropyl-2,5-dimethyl-1H-imidazole-4-carboxylate | HCID 45097089 | — |
反応手順
Fine powdered ammonium sulfate (0.13 g, 1 mmol) was added to a suspension of Z)-2-acetylamino-3-cyclopropylamino-but-2-enoic acid ethyl ester (7.0 g, 20 mmol) and hexamethyldisilazane (50 ml, 235 mmol) and refluxed over night at 145° C. The reaction mixture was evaporated and extracted with ethyl acetate and water. The organic phase was dried over sodium sulfate and evaporated. The crude product was purified by column chromatography on silica gel (ethyl acetate/methanol 4:1) and the desired compound was obtained as a light brown solid (1.3 g, 31%), MS: m/e=209.1 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07091222B2 |
|---|
| 出典データセット | uspto-grants-2006_08 |
|---|
| ORD ID | ord-ac2fb617a7cc49e7926340e6ef4fdd34 |
|---|
| 出典メモ | uspto-grants-2006_08 |
|---|