化工社化工社 化学情報印刷レポート · 研究参考用
Pyridine → HCID 12247535、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | 8-Azabicyclo(3.2.1)octane | HCID 136097 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 12247535 | HCID 12247535 | 70.3% |
反応手順
To a cooled (10° C.) solution 8-aza-bicyclo[3.2.1]octane (295 mg, 2.00 mmol) and pyridine (486 μL, 6.02 mmol) in DCM (10 mL) was added triphosgene (595 mg, 2.00 mmol) portionwise. The reaction was allowed to reach room temperature and stirred overnight. The mixture was quenched with HCl (1M aqueous, 10 mL) and stirred for 30 min. The aqueous phase was extracted with DCM (×3) and the combined organic layers were washed with HCl (1M aqueous), brine, dried (MgSO4) and concentrated in vacuo, to give the title compound (244 mg, 70%). 1H NMR (400 MHz, CDCl3): 1.46-1.70 (4H, m), 1.72-1.92 (5H, m), 2.04-2.11 (2H, m), 4.39-4.44 (2H, m).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08907094B2 |
| 出典データセット | uspto-grants-2014_12 |
| ORD ID | ord-7ef32beddf8b4b9586bb27c7e332323a |
| 出典メモ | uspto-grants-2014_12 |