関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Pyridine-2-carbonyl chloride | HCID 135034 | — |
| 反応物 | (3R)-1-[(4-chlorophenyl)sulfonyl]-3-methylpiperazine | HCID 11630465 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | (2R)-4-[(4-chlorophenyl)sulfonyl]-2-methyl-1-(2-pyridinylcarbonyl)piperazine | HCID 44612083 | 45.5% |
反応手順
To a solution of (3R)-1-[(4-chlorophenyl)sulfonyl]-3-methylpiperazine (0.15 g, 0.55 mmol) in dry acetonitrile (5 mL) was added potassium carbonate (90 mg, 0.66 mmol) and 2-pyridinecarbonyl chloride (106 mg, 0.60 mmol) and the reaction mixture heated at 85° C. for 24 h. To the mixture was added ethyl acetate (30 mL) and the organic phase washed with 10% aqueous sodium bicarbonate (50 mL) before it was dried (MgSO4), filtered and the solvent evaporated. The crude product was purified by Biotage SP4 (12+M silica column) eluting 0-4% MeOH in DCM to give the title compound as an off-white solid (95 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08530478B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-626bff4e6de04ebe8ef8b3da38d7a452 |
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| 出典メモ | uspto-grants-2013_09 |
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