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Ethyl Acetate → 3-(2-Bromoanilino)-4-(2-hydroxy-4-nitroanilino)-3-cyclobutene-1,2-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-Bromoaniline | HCID 11992 | — |
| 反応物 | 3-ethoxy-4-(2-Hydroxy-4-nitroanilino)-3-cyclobutene-1,2-dione | HCID 22238504 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 3-(2-Bromoanilino)-4-(2-hydroxy-4-nitroanilino)-3-cyclobutene-1,2-dione | HCID 10179343 | 19% |
反応手順
A solution of 3-ethoxy-4-(2-Hydroxy-4-nitroanilino)-3-cyclobutene-1,2-dione (0.39 g, 1.4 mmol) and 2-bromoaniline (0.36 g, 2.09 mmol) in 2 mL DMSO was heated at 110° C. for overnight. The reaction mixture was cooled to room temperature, and ethylacetate was added, and a precipitate formed. The filtrate was partitioned between ethylacetate and water. The organic layer was dried over sodium sulfate and concentrated. Titration from acetone and hexanes gave 106 mg (19%) of 3-(2-bromoanilino)-4-(2-hydroxy-4-nitroanilino)-3-cyclobutene-1,2-dione. LCMS(H+) 404
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07008962B2 |
| 出典データセット | uspto-grants-2006_03 |
| ORD ID | ord-d51b72e7d92f42fca638e17382a962f7 |
| 出典メモ | uspto-grants-2006_03 |