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Pyridine → (3-Bromothien-2-yl) (3-methoxyphenyl)methanone oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | (3-Bromothien-2-yl) (3-methoxyphenyl)methanone | HCID 21915416 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | (3-Bromothien-2-yl) (3-methoxyphenyl)methanone oxime | HCID 72727313 | 87% |
反応手順
Stir a mixture of (3-bromothiophen-2-yl)-(3-methoxyphenyl)methanone (7 g, 0.024 mol), hydroxylamine hydrochloride (3.09 g, 0.048 mol) and pyridine (40 mL) overnight at room temperature, and then heat the mixture (100° C.–105° C.) for four hours. TLC (dichloromethane) shows that the reaction is complete. Quench the reaction mixture with water and extract with ether (three times). Wash the ether phase with HCl (3N) and water, dry (MgSO4), filter and concentrate to yield an oil that solidifies. Recrystallize the solid from ether:hexane to obtain the title compound (6.4 g, 87% Yield), m.p. 102–103° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07125903B1 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-57b78ac06de9427ea6e74f79c1c384e6 |
| 出典メモ | uspto-grants-2006_10 |