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N,N-Dimethylaniline → ethyl (2Z)-2-(2-acetamido-1,3-thiazol-4-yl)-2-(2-oxopyrrolidin-3-yl)oxyiminoacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N-Dimethylaniline | HCID 949 | — |
| 反応物 | Acetylthiourea | HCID 2723593 | — |
| 反応物 | ethyl (2Z)-4-chloro-3-oxo-2-(2-oxopyrrolidin-3-yl)oxyiminobutanoate | HCID 13536861 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | ethyl (2Z)-2-(2-acetamido-1,3-thiazol-4-yl)-2-(2-oxopyrrolidin-3-yl)oxyiminoacetate | HCID 13536846 | 49.9% |
反応手順
2.77 g of ethyl (Z)-2-[(2-pyrrolidon-3-yl)oxyimino]-3-oxo-4-chloro-n-butyrate and 1.2 g of acetylthiourea are added to 20 ml of ethanol, and 2.0 g of N,N-dimethylaniline are added thereto. The mixture is stirred at 20° to 30° C. for 4 hours. Then, the mixture is concentrated under reduced pressure to drynss. The residue is dissolved in chloroform, and the solution is washed with water and an aqueous sodium bicarbonate solution, successively. The chloroform solution is dried and concentrated under reduced pressure to remove solvent. The residue is crystallized with isopropanol, and the crystals are collected by filtration. 1.7 g of ethyl (Z)-2-(2-acetamidothiazol-4-yl)-2-[(2-pyrrolidon-3-yl)oxyimino]acetate are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04794186 |
| 出典データセット | uspto-grants-1988_12 |
| ORD ID | ord-d6e50eb0df8941a9b773da1001eb169d |
| 出典メモ | uspto-grants-1988_12 |