関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Phenyl chloroformate | HCID 15891 | — |
| 反応物 | 5-Methoxypyridin-3-ylamine | HCID 12703595 | — |
| 生成物 | Phenyl 6-methoxypyridin-3-ylcarbamate | HCID 20185962 | 96% |
反応手順
3-Amino-5-methoxy-pyridine (5.00 g, 40.3 mmol) was dissolved in THF (80 mL), cooled to 0° C., treated with pyridine (4.07 mL, 50.4 mmol) followed by phenylchloroformate (5.32 mL, 42.3 mmol). The reaction mixture was slowly warmed to RT over several hours and stirred an additional 12 h. The mixture was partitioned between water and EtOAc. The organic layer was separated and the aqueous layer was extracted again. The combined organic extracts were dried over sodium sulfate, filtered and concentrated to give the product as a reddish solid (9.45 g, 96%), which was used without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08044052B2 |
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| 出典データセット | uspto-grants-2011_10 |
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| ORD ID | ord-bf15aa18ac8640bd9f5cd0e1d19e0ffa |
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| 出典メモ | uspto-grants-2011_10 |
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