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Hydrochloric Acid → 2-(2-Isopropylthiopyrid-3-yloxy)-propionic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Methyl 2-bromopropionate | HCID 95576 | — |
| 反応物 | 3-Pyridinol, 2-[(1-methylethyl)thio]- | HCID 19957932 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-(2-Isopropylthiopyrid-3-yloxy)-propionic acid methyl ester | HCID 54493063 | — |
反応手順
12.3 ml of 2-bromopropionic acid methyl ester are added dropwise at room temperature to a mixture of 16.9 g of 2-isopropylthio-3-hydroxypyridine and 15.2 g of potassium carbonate in 250 ml of dimethylformamide and the batch is stirred for 75 minutes. The suspension is introduced into a mixture of ice-water (300 ml), 50 ml of 2N hydrochloric acid and 300 ml of ethyl acetate, washed four times with 120 ml of water and 120 ml of ethyl acetate each time, and the organic phase is dried over sodium sulfate and concentrated by evaporation. 25.4 g of the desired intermediate are obtained in the form of a viscous oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05625071 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-cb746f3e77cc4c7ca2fa00427cf9c504 |
| 出典メモ | uspto-grants-1997_04 |