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Hydrochloric Acid → 5-(2,2-Difluorovinyl)-N-methyl-N-propyl-isophthalamic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | 5-(2,2-Difluorovinyl)-N-methyl-N-propyl-isophthalamic acid ethyl ester | HCID 68814519 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 5-(2,2-Difluorovinyl)-N-methyl-N-propyl-isophthalamic acid | HCID 68814040 | 44% |
反応手順
Stir a solution of 5-(2,2-difluorovinyl)-N-methyl-N-propyl-isophthalamic acid ethyl ester (187 mg, 0.63 mmol), 1 N lithium hydroxide (2.5 mL, 2.5 mmol) and THF (2.5 mL) at room temperature overnight. Partition the reaction between ethyl acetate and water. Acidify the aqueous with 5 N HCl and extract with ethyl acetate. Dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 2:98 to 6:94 methanol:dichloromethane with 1% acetic acid) to give the title compound (78 mg, 44%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07585885B2 |
| 出典データセット | uspto-grants-2009_09 |
| ORD ID | ord-742e24919a8547b198ae5de791cb4012 |
| 出典メモ | uspto-grants-2009_09 |