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2-(Dimethylamino)acetyl chloride hydrochloride → N-(6-iodoimidazo[1,2-b]pyridazin-2-yl)-N2,N2-dimethylglycinamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(Dimethylamino)acetyl chloride hydrochloride | HCID 13994991 | — |
| 反応物 | 6-Iodoimidazo[1,2-B]pyridazin-2-amine | HCID 57441024 | — |
| 溶媒 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | N-(6-iodoimidazo[1,2-b]pyridazin-2-yl)-N2,N2-dimethylglycinamide | HCID 57708588 | 74% |
反応手順
To a solution of 6-iodoimidazo[1,2-b]pyridazin-2-amine (1040 mg, 4.0 mmol) in N-methylpyrrolidone (5.0 mL) was added dimethylaminoacetyl chloride hydrochloride (948 mg, 6.0 mmol), and the mixture was stirred at room temperature for 6 hr. The reaction mixture was diluted with 1N aqueous sodium hydroxide solution, and extracted with ethyl acetate. The organic layer was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/methanol=100/0→70/30), and precipitated from diisopropyl ether to give the title compound (1019 mg, 74%) as a pale-yellow 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-ab7e303991a24e528d74da727176acc4 |
| 出典メモ | uspto-grants-2012_09 |