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Triethylamine → HCID 59764775、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-(Isocyanatomethyl)-4-methylbenzene | HCID 2733388 | — |
| 反応物 | 4-Phenyl-1-pyrrolidin-3-yl-piperidine dihydrochloride | HCID 68899888 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 59764775 | HCID 59764775 | 68% |
反応手順
To a solution of 4-phenyl-1-pyrrolidin-3-yl-piperidine dihydrochloride (preparation #7) (0.050 g, 0.165 mmol) and triethylamine (0.092 mL, 0.66 mmol) in dichloromethane (1 mL) was added 1-isocyanatomethyl-4-methyl-benzene (0.024 g, 0.165 mmol) and the reaction mixture was stirred at ambient temperature for about 16 h. The reaction mixture was concentrated in vacuo and the residue was purified by flash chromatography on silica gel using 5% MeOH/EtOAc as the mobile phase to give 3-(4-phenyl-piperidin-1-yl)-pyrrolidine-1-carboxylic acid 4-methyl-benzylamide (0.042 g, 68%). RP-HPLC (Table 1, Method b) Rt 1.72 min; m/z: (M+H)+ 378.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08754107B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-28fcf59ea7be42fda0561fec2ceba150 |
| 出典メモ | uspto-grants-2014_06 |