참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Pyridine-2-carbonyl chloride | HCID 135034 | — |
| 반응물 | (3R)-1-[(4-chlorophenyl)sulfonyl]-3-methylpiperazine | HCID 11630465 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | (2R)-4-[(4-chlorophenyl)sulfonyl]-2-methyl-1-(2-pyridinylcarbonyl)piperazine | HCID 44612083 | 45.5% |
반응 단계
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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08530478B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-626bff4e6de04ebe8ef8b3da38d7a452 |
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| 출처 메모 | uspto-grants-2013_09 |
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