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Chloroform → Methyl 3-(2-piperidinyl)propanoate hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Methyl 3-(2-pyridyl)-2-propenoate | HCID 53733726 | — |
| 触媒 | Adams' catalyst | HCID 345198 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Methyl 3-(2-piperidinyl)propanoate hydrochloride | HCID 47000747 | — |
反応手順
Methyl 3-(pyridin-2-yl)acrylate (22.15 g, 136 mmol) was dissolved in THF (300 ml) and chloroform (10.9 ml), and PtO2 (3.08 g, 13.6 mmol, 0.1 eq.) was added under a nitrogen atmosphere. The solution was first rinsed with nitrogen for 10 min and was then stirred overnight under a H2 atmosphere (8 bar). After cooling, rinsing with nitrogen was first carried out again, the catalyst was removed by filtering over filtering earth and then rinsed with DCM, and the filtrate was concentrated to dryness in vacuo. The methyl 3-(piperidin-2-yl)propionate hydrochloride was used in the next stage without being purified further.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08124624B2 |
| 出典データセット | uspto-grants-2012_02 |
| ORD ID | ord-71c88d92b1124036883e326911ef9ce3 |
| 出典メモ | uspto-grants-2012_02 |