참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Piperazine | HCID 4837 | — |
| 반응물 | 3-Bromopyridine | HCID 12286 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | O-Xylene | HCID 7237 | — |
| 생성물 | 1-(Pyridin-3-yl)piperazine | HCID 437234 | 86% |
반응 단계
A 500 ml Kjeldahl flask equipped with a cooling condenser and a thermometer was charged with a solution of 44.6 g of piperazine in 45 ml of o-xylene, a solution of 13.44 g of 3-bromopyridine in 45 ml of o-xylene, and a solution of 11.3 g of NaOBut in 45 ml of o-xylene, and further with a solution of 19 mg of palladium acetate in 10 ml of o-xylene (the ratio of palladium atom/heterocyclic aromatic halide=0.1% by mole). The flask was flushed with nitrogen for about 20 minutes while the content was stirred, and 0.26 ml of a solution in toluene of tri-tert.-butylphosphine having a concentration of 0.256 g/ml was added. Then the mixture was heated to 120° C., and maintained at that temperature for 3 hours with stirring. After completion of the reaction, the same treatment as employed in Example 1 was conducted to give colorless oily 1-(3-pyridyl)piperazine. The yield was 86% by mole.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05929281 |
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| 출처 데이터셋 | uspto-grants-1999_07 |
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| ORD ID | ord-846733b7bf3242d4afa79aeadbf31362 |
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| 출처 메모 | uspto-grants-1999_07 |
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