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2-Propanone, 1-(acetyloxy)-3-chloro- → (6-Iodoimidazo[1,2-b]pyridazin-2-yl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Propanone, 1-(acetyloxy)-3-chloro- | HCID 38413 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 6-Iodopyridazin-3-amine | HCID 10867834 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (6-Iodoimidazo[1,2-b]pyridazin-2-yl)methanol | HCID 57441048 | 20.1% |
反応手順
To a solution of 3-amino-6-iodopyridazine (2.0 g, 9.0 mmol) in ethanol (40 mL) was added 3-chloro-2-oxopropyl acetate (2.73 g, 18.1 mmol), and the mixture was heated under reflux for 24 hr. After cooling the mixture to room temperature, saturated aqueous sodium hydrogencarbonate solution was added to the mixture, and the mixture was extracted with ethyl acetate/tetrahydrofuran. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and filtrated. The solvent was evaporated under reduced pressure, and the residue was collected by filtration and washed with ethyl acetate/hexane to give the title compound (498 mg, 20%) as a white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08273741B2 |
| 出典データセット | uspto-grants-2012_09 |
| ORD ID | ord-fb36066fc9494afc8093712a96d14709 |
| 出典メモ | uspto-grants-2012_09 |