化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dichloroethane → 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl 4-piperidinecarboxylate | HCID 70770 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 1-Methylcyclopropanecarboxylic acid | HCID 81326 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(1-Methyl-cyclopropanecarbonyl)-piperidine-4-carboxylic acid ethyl ester | HCID 59438144 | 92% |
反応手順
To a stirred solution of 1-methyl-cyclopropanecarboxylic acid (14.4 g, 0.144 mol) in 200 mL of CH2Cl2 was added (27.10 g, 0.141 mol) of EDC, (19.10 g, 0.141 g) of HOBt and Et3N (35.93 mL, 0.259 mol). After one hour at RT, was added piperidine-4-carboxylic acid ethyl ester (18.90 g, 0.120 mol). The mixture was stirred at RT over night and then poured onto water and extracted with CH2Cl2. The combined organic phases were dried over Na2SO4 and concentrated under vacuo. Column chromatography (SiO2, EtOAc/H, 1:1) yielded 26.1 g (92%) of the title compound as a light yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08063075B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-a1872268c8804dbea2cad75708340c6e |
| 出典メモ | uspto-grants-2011_11 |