関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 1-Methyl-1H-pyrazole-3-sulfonyl chloride | HCID 13474466 | — |
| 反応物 | 6-benzylamino-3,4-dihydro-2H-isoquinolin-1-one | HCID 67223915 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-methyl-1H-pyrazole-3-sulfonic acid benzyl-(1-oxo-1,2,3,4-tetrahydro-isoquinolin-6-yl)-amide | HCID 67223998 | 14% |
反応手順
To a stirred solution of 6-benzylamino-3,4-dihydro-2H-isoquinolin-1-one (45 mg, 0.18 mmol) and pyridine (31 μl, 0.39 mmol) in anhydrous acetonitrile (1 ml) was added 1-methyl-1H-pyrazole-3-sulfonyl chloride (70 mg, 0.39 mmol) and the reaction heated to 150° C. in a microwave for 0.5 hrs. The solvent was evaporated in vacuo and the crude residue purified by preparative tlc (5% methanol in dichloromethane) to afford the title compound as a yellow solid (10 mg, 14%). HPLC retention time 3.83 min. Mass spectrum (ES+) m/z 397 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08399481B2 |
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| 出典データセット | uspto-grants-2013_03 |
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| ORD ID | ord-c56c91d3a32c4bb49b4d22546a0e637f |
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| 出典メモ | uspto-grants-2013_03 |
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