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Bromoacetone → 6-Chloro-2,8-dimethyl-imidazo[1,2-b]pyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromoacetone | HCID 11715 | — |
| 反応物 | 6-Chloro-4-methylpyridazin-3-amine | HCID 12353664 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 6-Chloro-2,8-dimethyl-imidazo[1,2-b]pyridazine | HCID 12248340 | — |
反応手順
3-Amino-6-chloro-4-methylpyridazine (5.50 g, 38.3 mmol) and bromoacetone (6.90 g, 40.0 mmol) were heated in acetonitrile (50.0 ml) for 8 hours under reflux. The reaction solution was concentrated under reduced pressure, and water (100 ml) was added to the residues which were then adjusted to pH 9 with 20% aqueous sodium hydroxide and extracted twice with ethyl acetate. The extracts were combined, dried over anhydrous magnesium sulfate and concentrated, and the residues were purified by silica gel column chromatography (ethyl acetate:chloroform=1:2), to give the title compound as white crystals. The yield was 3.80 g (54.6%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07816526B2 |
| 出典データセット | uspto-grants-2010_10 |
| ORD ID | ord-990a68adc2e24486b262b7c0eb65937f |
| 出典メモ | uspto-grants-2010_10 |