関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | [1-(2,4-difluoro-phenyl)-6-methoxy-isoquinolin-3-yl]-(5-methyl-1H-pyrazol-3-yl)-amine | HCID 23633788 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | HCID 136055524 | HCID 136055524 | 8.7% |
反応手順
To a solution of [1-(2,4-difluoro-phenyl)-6-methoxy-isoquinolin-3-yl]-(5-methyl-1H-pyrazol-3-yl)-amine (11.0 g) in 10 mL acetic acid was added hydrobromic acid (1 mL, 40%). The mixture was heated at 180° C. for 30 min under microwave irradiation. After cooling, most of the solvent was removed under reduced pressure, the residue was dissolved in 100 mL of ethyl acetate and washed with saturated sodium bicarbonate. The organic phase was dried with anhydrous sodium sulfate and concentrated to give an oil (0.92 g), which was used for the next reaction without further purification. (LC-MS m/e 353 MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07572809B2 |
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| 出典データセット | uspto-grants-2009_08 |
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| ORD ID | ord-651daadcade84d478828c1227c5f054e |
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| 出典メモ | uspto-grants-2009_08 |
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