참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1-Methylpiperazine | HCID 53167 | — |
| 반응물 | 5-Bromo-2-nitropyridine | HCID 817620 | — |
| 촉매 | Tetrabutylammonium Iodide | HCID 67553 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 1-Methyl-4-(6-nitropyridin-3-yl)piperazine | HCID 51711484 | 83.1% |
반응 단계
To 5-Bromo-2-nitro-pyridine (2.00 g, 9.85 mmol) in 10 mL dimethylsulfoxide was added potassium carbonate (2.72 g, 19.7 mmol), 1-methylpiperazine (1.64 mL, 14.8 mmol), and tetrabutylammonium iodide (36 mg, 0.097 mmol) and was heated at 120° C. for 18 hours. The mixture was made acidic with 1M aq. HCl and was partitioned between dichloromethane and water. The aqueous layer was made basic with 2M aq. sodium carbonate and was extracted with dichloromethane. The organic layer was dried over anhydrous magnesium sulfate, concentrated in vacuo, and was triturated with water to yield 1-Methyl-4-(6-nitro-pyridin-3-yl)-piperazine (1.82 g, 8.19 mmol). MS (ESI) 223.1 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08822457B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
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| ORD ID | ord-39e811d8cd514cef8227c892e3909540 |
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| 출처 메모 | uspto-grants-2014_09 |
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