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Formaldehyde → 6-Methylnicotine, (A+-)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Methyl-5-(pyrrolidin-2-yl)pyridine | HCID 12749684 | — |
| 溶媒 | Formic Acid | HCID 284 | — |
| 生成物 | 6-Methylnicotine, (A+-)- | HCID 5020711 | 92% |
反応手順
Into a round bottom flask was placed XVI (2.0 g), and formaldehyde (37% w/v in water, 20 mL) and formic acid (95-97% w/v, 45 mL), both a 0° C., were added. The mixture then was refluxed under nitrogen for 8 hr. The cooled reaction mixture was basified with aqueous sodium hydroxide (50% w/v) to pH 8-9, and the solution extracted with chloroform (5×25 mL). The combined organic liquors were dried over anhydrous sodium sulfate, filtered and evaporated; and the resulting oil distilled under reduced pressure to afford XVII as a clear odorless oil (b.p. 107° C. at 3 mm Hg, 92% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726316 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-acfd98fbecaf4acda872324b5f557a19 |
| 出典メモ | uspto-grants-1998_03 |