関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | 6-Iodoimidazo[1,2-B]pyridazin-2-amine | HCID 57441024 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(6-iodoimidazo[1,2-b]pyridazin-2-yl)acetamide | HCID 57441059 | — |
反応手順
To a 50-mL round bottom flask was added 6-iodo-imidazo[1,2-b]pyridazin-2-ylamine (130 mg, 0.5 mmol, 1 eq), anhydrous dichloromethane (10 mL), acetic anhydride (0.071 mL, 1.5 eq), pyridine (0.073 mL, 1.8 eq), and 4-(dimethylamino)pyridine (0.61 mg, 0.01 eq). After the mixture was stirred at room temperature for four hours, it was quenched with saturated aqueous sodium bicarbonate and extracted with i-PrOH—CHCl3 (1:4). The organic layer was isolated, washed with brine, and dried with anhydrous sodium sulfate. The upper clear solution was decanted, concentrated, and the residue was subject to a gradient column chromatography (from DCM to MeOH-DCM 1:30) to yield N-(6-iodoimidazo[1,2-b]pyridazin-2-yl)acetamide as a white solid in amount of 67 mg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09233968B1 |
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| 出典データセット | uspto-grants-2016_01 |
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| ORD ID | ord-ea3d1294d6934a98a922f30fb7b59a34 |
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| 出典メモ | uspto-grants-2016_01 |
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