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Formic Acid → (1-Methyl-3-piperidyl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Piperidin-3-ylmethanol | HCID 107308 | — |
| 生成物 | (1-Methyl-3-piperidyl)methanol | HCID 97998 | 76.1% |
反応手順
A! At 0° C., 3-hydroxymethyl-piperidine (20 g, 173 mmoles) was slowly added to formic acid (63 ml, 1.66 moles) then a 40% solution of formaldehyde was added (62.4 ml, 833 mmoles). The mixture was refluxed for 5 hours, then the solvent was evaporated and the residue taken up in little water, brought to basic pH with 32% sodium hydroxide and extracted with ethyl ether. The organic phase was anhydrified over sodium sulfate and evaporated. The resultant crude was purified by distillation and provided 17 g (yield: 76%) of N-methyl-3-hydroxymethylpiperidine (b.p.--85°-86° C./1 mmHg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05827881 |
| 出典データセット | uspto-grants-1998_10 |
| ORD ID | ord-68a2ee096080469aa9ade94c557ef8e8 |
| 出典メモ | uspto-grants-1998_10 |