関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl 4-piperidinecarboxylate | HCID 70770 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Bromo-4-methylpyridine | HCID 2734087 | — |
| 溶媒 | 3-(3-Methoxypropoxy)-1-propanol | HCID 66984 | — |
| 生成物 | Ethyl 1-(4-methyl-2-pyridyl)piperidine-4-carboxylate | HCID 62007359 | 56% |
反応手順
2-Bromo-4-methylpyridine (860 mg, 5 mmol), ethyl piperidine-4-carboxylate (865 mg, 5.5 mmol) and DIPEA (958 μl, 5.5 mmol) were mixed in dipropyleneglycolmonomethylether (10 ml) and stirred at 150° C. overnight. Additional ethyl piperidine-4-carboxylate (865 mg, 5.5 mmol) was added and stirring was continued at 150° C. for 24 hours. The mixture was concentrated under reduced pressure and the residue was purified by column chromatography (silica, gradient from 0 to 30% ethyl acetate in DCM) to give 700 mg of a brown solid (2.8 mmol, 56%) MS (multi-mode) m/z=249.1 [M+1]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09260441B2 |
|---|
| 出典データセット | uspto-grants-2016_02 |
|---|
| ORD ID | ord-4094ab713b40481c8bd9863b0bf14f04 |
|---|
| 出典メモ | uspto-grants-2016_02 |
|---|
