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2-Propen-1-one, 3-(dimethylamino)-1-(4-pyridinyl)- → 2-Methyl-7-(4-pyridinyl)pyrazolo(1,5-a) pyrimidine-3-carbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Propen-1-one, 3-(dimethylamino)-1-(4-pyridinyl)- | HCID 714531 | — |
| 反応物 | HCID 178434678 | HCID 178434678 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2-Methyl-7-(4-pyridinyl)pyrazolo(1,5-a) pyrimidine-3-carbonitrile | HCID 15042079 | 52.5% |
反応手順
A mixture of 6.1 g of 5-amino-3-methyl-4-pyrazole carbonitrile and 8.81 g of 3-dimethylamino-1-(4-pyridinyl)-2-propen-1-one in 50 ml of glacial acetic acid is stirred and heated at reflux for 5 hours. The reaction mixture is cooled and the precipitate which forms is collected by filtration and washed with water and a little dichloromethane to give a solid. The solid is partitioned between saturated sodium bicarbonate and dichloromethane. The organic layer is dried over anhydrous sodium sulfate and passed through a short column of hydrous magensium silicate. The addition of hexane to the eluate crystallizes the product which is collected by filtration to give 6.17 g of the desired product, mp 220°-221° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05059691 |
| 出典データセット | uspto-grants-1991_10 |
| ORD ID | ord-736be818a20d44ff905cd66d42aed486 |
| 出典メモ | uspto-grants-1991_10 |