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Hydrochloric Acid → 2-(6,7-Dichloroisatin-1-yl)acetic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl bromoacetate | HCID 7748 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 5,6-dichloro-1H-indole-2,3-dione | HCID 11009341 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(6,7-Dichloroisatin-1-yl)acetic acid | HCID 22274383 | 67% |
反応手順
A solution of 5,6-dichloroisatin (1.0 g, 4.65 mmol) in DMF (20 ml) was cooled in an ice-bath. Sodium hydride (5.11 mmol, 0.20 g 60% dispersion in mineral oil) was added and the mixture was stirred for 20 min. Ethyl 2-bromoacetate (0.37 ml, 5.11 mmol) was added and stirring was continued for 2 hours. The resulting mixture was poured into diluted hydrochloric acid (200 ml, 4M), heated to reflux for 2 hours, filtered, cooled and extracted with ethyl acetate. The organic extract was dried over magnesium sulphate and evaporated to dryness to leave the desired product (0.85 g, 67%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06969729B2 |
| 出典データセット | uspto-grants-2005_11 |
| ORD ID | ord-a256b6b2ea684138a22a5720350a25d6 |
| 出典メモ | uspto-grants-2005_11 |