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Water → 2-acryloylamino-5-[pyridazin-3(2H)-on-6-yl]indane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Acryloyl chloride | HCID 13140 | — |
| 反応物 | 2-amino-5-[pyridazin-3(2H)-on-6-yl]indane hydrobromide | HCID 18929772 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-acryloylamino-5-[pyridazin-3(2H)-on-6-yl]indane | HCID 19972854 | 80.4% |
反応手順
Under ice cooling, 3.0 g of acryloyl chloride dissolved in 50 ml of tetrahydrofuran was added dropwise to a suspension of 5.03 g of 2-amino-5-[pyridazin-3(2H)-on-6-yl]indane·hydrobromide in 150 ml of ethyl acetate and 150 ml of water containing 4.52 g of potassium carbonate, and the mixture was stirred for 3 hours. Crystals precipitated were collected by filtration, washed with water, dried and then recrystallized from methanol-acetonitrile to obtain 3.69 g of 2-acryloylamino-5-[pyridazin-3(2H)-on-6-yl]indane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05543409 |
| 出典データセット | uspto-grants-1996_08 |
| ORD ID | ord-99af5a186c2e40ba956f8123a329b311 |
| 出典メモ | uspto-grants-1996_08 |