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Hydrochloric Acid → 4-(3-chloro-6-pyridazinyloxy)phenylacetic Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Phenylacetic Acid | HCID 999 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Pyridazine | HCID 9259 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 生成物 | 4-(3-chloro-6-pyridazinyloxy)phenylacetic Acid | HCID 23353621 | — |
反応手順
To a mixture of 0.54 g (0.013 mol, 2.0 equiv) of 60% sodium hydride/mineral oil dispersion in 10 m of dry DMF was added dropwise at room temperature a solution 1.02 g (0.0067 mol) of the phenylacetic acid in 2.3 mL of DMF. After 15-20 minutes, a solid existed which was difficult to stir. The pyridazine (1.0 g, 0.0067 mol) was then added and the mixture was heated at 60°-65° C. for about 2 hours and was allowed to cool. The mixture was poured onto ice water and was adjusted to pH 5 with 2.0N HCl, and the precipitate was collected. This material was triturated under heptane to afford 880 mg of the title product. MP 124°-127° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05597836 |
| 出典データセット | uspto-grants-1997_01 |
| ORD ID | ord-7aba8952b0c94c119cf98a1868fbe356 |
| 出典メモ | uspto-grants-1997_01 |