関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Dibromopropane | HCID 8001 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-Amino-4-cyanopyrazole | HCID 85515 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4,5,6,7-Tetrahydropyrazolo[1,5-a]pyrimidine-3-carbonitrile | HCID 135671372 | — |
反応手順
To a solution of 5-aminopyrazole-4-carbonitrile (102 g) and triethylamine (316 ml) in 1,4-dioxane (2000 ml) was added 1,3-dibromopropane (115 ml), and the mixture was stirred at 95° C. for 5 days. The insoluble materials were removed by filtration, and the filtrate was concentrated in vacuo. To the residue was added 10% aqueous citric acid solution, and the mixture was extracted with chloroform. The extract was dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo. The residue was triturated with 2-propanol and dried in vacuo to give 4,5,6,7-tetrahydropyrazolo[1,5-a]pyrimidine-3-carbonitrile (8.0 g) as a solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07179801B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-912c718fea374522827ed71adc7db813 |
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| 出典メモ | uspto-grants-2007_02 |
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