関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Diphenyl N-Cyanocarbonimidate | HCID 688090 | — |
| 反応物 | (3r,4s)-4-((r)-3-Phenyl-pyrrolidine-1-carbonyl)-piperidine-3-carboxylic acid methyl ester | HCID 67304902 | — |
| 生成物 | HCID 178501357 | HCID 178501357 | 88.2% |
反応手順
To a stirred solution of (3R,4S)-4-((R)-3-Phenyl-pyrrolidine-1-carbonyl)-piperidine-3-carboxylic acid methyl ester (654 mg, 0.00207 mol) in anhydrous acetonitrile (11.0 mL, 0.211 mol) at rt was added triethylamine (0.579 mL, 0.00413 mol) and diphenyl cyanocarbonimidate (762 mg, 0.00310 mol). The reaction mixture was heated to reflux (oil bath temperature: 85° C.) for 18 h. The reaction mixture was concentrated in vacuo. The residue was purified by Combiflash with 40-90% EtOAc/Hex to give the product as a colorless solid (841 mg, 88% in yield). MS (ESI): (M+H)+=461.1.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08853243B2 |
|---|
| 出典データセット | uspto-grants-2014_10 |
|---|
| ORD ID | ord-3985aa424dd74423a910ecf8e93e496a |
|---|
| 出典メモ | uspto-grants-2014_10 |
|---|
