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4-Aminopyridine → Carbamic acid, 4-pyridinyl-, phenyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Aminopyridine | HCID 1727 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Carbamic acid, 4-pyridinyl-, phenyl ester | HCID 11401617 | 78.4% |
反応手順
To a solution of phenyl chloroformate (5.64 g) in dichloromethane (70 ml) was added a solution of 4-aminopyridine (2.84 g) and triethylamine (5.02 ml) in dichloromethane (100 ml) dropwise under cooling on an ice-water bath. After stirring for 1 hour, the solvents were removed under reduced pressure. A residue was diluted with dichloromethane (200 ml) and water (200 ml). An organic phase was separated and washed with water and brine. After drying with magnesium sulfate, the solvents were removed under reduced pressure. The reaction mixture was diluted with diisopropyl ether and the precipitates were filtered. After rinse with diethyl ether, O-phenyl N-(4-pyridyl)carbamate (5.07 g) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06710043B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-9dacb9240a3644f7b68c0ff696ee87d3 |
| 出典メモ | uspto-grants-2004_03 |