関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | (1-Chloro-7-fluoro-6-methoxy-isoquinolin-3-yl)-(5-methyl-1H-pyrazol-3-yl)-amine | HCID 57799484 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-Bromo-7-fluoro-3-(5-methyl-1H-pyrazol-3-ylamino)-isoquinolin-6-ol | HCID 136055525 | — |
反応手順
To a solution of (1-Chloro-7-fluoro-6-methoxy-isoquinolin-3-yl)-(5-methyl-1H-pyrazol-3-yl)-amine (1.0 g) in 10 mL acetic acid was added hydrobromic acid (1 mL, 40%). The mixture was heated at 160° C. for 30 min under microwave irradiation. Most of the solvent was removed under reduced pressure, and the residue was dissolved in 100 mL of ethyl acetate and washed with saturated sodium bicarbonate. The organic layer was dried with anhydrous sodium sulfate and concentrated to give oil (0.92 g), which was used for the next reaction without further purification. LC-MS m/e 338 (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-f05aaaed1c3d4971a1f35e4749ef0c8c |
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| 出典メモ | uspto-grants-2009_08 |
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