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Triethylamine → HCID 9956174、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | N,N-Dimethylethylenediamine | HCID 66053 | — |
| 反応物 | 5-Methylthio-6-trifluoromethyl-1-(3-carboxy Phenyl Carbamoyl)indoline | HCID 18005107 | — |
| 触媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 9956174 | HCID 9956174 | 45% |
反応手順
To a suspension of 5-methylthio-6-trifluoromethyl-1-(3-carboxy phenyl carbamoyl) indoline (0.5 g, 1.26mmol) in dichloromethane (20 ml) was added oxalyl chloride (0.3 ml, 2.52 mmol) and dimethylformamide (3 drops). After effervescing had subsided the reaction mixture was evaporated to dryness under reduced pressure. It was then dissolved in tetrahydrofuran (30 ml) and added to a solution of N,N-dimethylethylenediamine (0.405 g, 6.33mmol) and triethylamine (0.2 ml, 1.4 mmol) in tetrahydrofuran at 0° C. After 2 hours the reaction mixture was basified with 5M NaOH and water was added forming a white precipitate. This was filtered and dried to give the product a white solid (0.25 g, 45%), m.p. 91-93° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05972937 |
| 出典データセット | uspto-grants-1999_10 |
| ORD ID | ord-f8280e4dd96b47f9a1c79f68bf4aa884 |
| 出典メモ | uspto-grants-1999_10 |