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Methyl 5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinate → 5-Chloro-2-(2-phenylpyrrolidin-1-yl)nicotinic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinate | HCID 67958237 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 5-Chloro-2-(2-phenylpyrrolidin-1-yl)nicotinic acid | HCID 67958697 | 108% |
反応手順
To an ice cooled solution of methyl 5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinate (D72) (165 mg, 0.520 mmol) in methanol (10 ml), 10N NaOH (10 ml) was added. The mixture was heated under reflux overnight. After cooled to room temperature, the mixture was concentrated in vacuo. The residue was diluted with water (10 ml), acidified with 2.5N HCl (pH 1-2), and the resulting mixture was extracted with ethyl acetate (2×10 ml). The organic solution was washed with brine (20 ml), dried over Na2SO4 and evaporated in vacuo to afford the title compound (D98) (170 mg) as a red solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08828987B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-81d088ce54304cf29e2e7ba529ec83ca |
| 出典メモ | uspto-grants-2014_09 |