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Methanol → 3-Pyridineacetic acid, ethyl ester, 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | Ethyl 3-pyridylacetate | HCID 96490 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 3-Pyridineacetic acid, ethyl ester, 1-oxide | HCID 4210360 | 124.9% |
反応手順
m-Chloro perbenzoic acid (6.2 g, 36.06 mmol) in CHCl3 (30 mL) was added drop wise to a solution of ethyl 2-(pyridin-3-yl)acetate (3.5 g, 21.21 mmol) in CHCl3 (30 mL) at room temperature under nitrogen atmosphere and the resulting reaction mass was stirred at room temperature for 5 hours. The reaction was monitored by TLC (10% methanol in chloroform). The reaction mass was basified using aqueous NaHCO3 solution to pH 7 and extracted using CHCl3. The organic layer was dried over sodium sulphate and concentrated under reduced pressure to afford 4.8 g of the crude product. LCMS: 60.09%, m/z=182.0 (M+1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08946260B2 |
| 出典データセット | uspto-grants-2015_02 |
| ORD ID | ord-687397d066c243679035f1b64c09f428 |
| 出典メモ | uspto-grants-2015_02 |