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Water → Phenyl 6-methoxypyridin-3-ylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 6-Methoxy-3-pyridinylamine | HCID 81121 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Phenyl 6-methoxypyridin-3-ylcarbamate | HCID 20185962 | — |
反応手順
6-Methoxy-pyridin-3-ylamine (1.0 g, 8.06 mmol) and pyridine (18 ml) are stirred in dry CH2Cl2. To this mixture phenylchloroformate (1.9 g, 12.0 mmol) is added and stirred for 24 hours at room temperature. Water and a solution of 1:1 EtOAc/hexanes is added to the mixture and the organic layer is separated. The organic layer is washed with 1N HCl three times and with brine once. The organic layer is dried over Na2SO4, filtered, and evaporated in vacuo. Purify by flash column chromatography (0-10% EtOAc/CH2Cl2) to obtain (6-methoxy-pyridin-3-yl)-carbamic acid phenyl ester. Mass spec.: m+1=245 (AP+)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06566367B2 |
| 出典データセット | uspto-grants-2003_05 |
| ORD ID | ord-3cbdfa93dbb24b87a0629322df48f552 |
| 出典メモ | uspto-grants-2003_05 |