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4,4'-Bipyridine → 4,4'-Bipyridine, 1-oxide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4,4'-Bipyridine | HCID 11107 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4,4'-Bipyridine, 1-oxide | HCID 12299154 | — |
反応手順
To the solution of 4,4′-bipyridine (25.00 g, 160.08 mmol, 1 equiv) in CH2Cl2 (200 mL) at 0° C. was added 3-chloroperoxybenzoic acid (35.87 g, 77%, 160.06 mmol, 1 equiv). The reaction mixture was stirred overnight at rt. The solid was filtered off and the filtrate was concentrated and purified by flash column chromatography (acetone to 10% MeOH in acetone) to give 4,4′-bipyridine-1-oxide (3-1) as a solid. 1H NMR (CDCl3) δ 8.75 (d, 2H, J=5.9), 8.31 (d, 2H, J=7.1), 7.57 (d, 2H, J=7.0), 7.50(d, 2H, J=6.1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07125888B2 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-b8430c7f54844990adc07339a8c4c2e7 |
| 出典メモ | uspto-grants-2006_10 |