関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,4-Diazabicyclo(3.2.2)nonane | HCID 398407 | — |
| 反応物 | HCID 178419486 | HCID 178419486 | — |
| 触媒 | HCID 178479802 | HCID 178479802 | — |
| 生成物 | 3-(1,4,Diazabicyclo[3.2.2]non-4-ylcarbonyl)-1h-pyrazolo[3,4-c]pyridine | HCID 68968013 | — |
反応手順
1 g (5 mmol) of 3-bromo-1H-pyrazolo[3,4-c]-pyridine, 0.53 g (0.75 mmol) of bis(triphenylphosphino)dichloropalladium, 1.9 g (15.1 mmol) of 1,4-diazabicyclo[3.2.2]nonane and 3.5 ml (25 mmol) of triethylamine dissolved in 15 ml of N,N-dimethylformamide are successively introduced into a 50 ml reactor. The mixture is then purged with carbon monoxide and heated at 110° C. for 20 hours. The reaction medium is poured into 100 ml of water and the aqueous phase is extracted with chloroform. After drying the organic phases, they are dried, filtered and concentrated under reduced pressure. The residue is purified by chromatography on a column of silica gel, eluting with a mixture of chloroform, methanol and aqueous ammonia in 90/10/1 proportions.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524706B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-814e87e08ebe42e0a69e2333a633230c |
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| 出典メモ | uspto-grants-2013_09 |
|---|