참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Pyrazine, 2-phenyl- | HCID 642870 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-Phenylpiperazine | HCID 250673 | 59.5% |
반응 단계
To a solution of 2-phenylpyrazine (11.64 g, 74.53 mmol) in acetic acid (58.2 mL) was added palladium acetate Pd(OAc)2 (2.33 g, 9.94 mmol). The mixture was hydrogenated at 50 psi for 4 h. After the reaction was complete, the catalyst was filtered off and rinsed with a small portion of acetic acid. The filtrate was concentrated under house vacuum to give a brown-black solid which was suspended in deionized water (300 mL) and adjusted to pH 13 with 20% NaOH solution. The product was extracted from aqueous solution with EtOAc (200 mL, 3×), dried over MgSO4, filtered and evaporated to dryness to give 2-phenylpiperazine (7.2 g). An additional 1.6 g of 2-phenylpiperazine was obtained by evaporating the aqueous fraction to a solid and triturating the solid with CH2Cl2. Total yield of 2-phenyl-piperazine was 73%. The crude material was crystallized from EtOAc and hexane for characterization, m.p. 86°-88° C.; FAB MS [M+1]+ 163;
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05892039 |
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| 출처 데이터셋 | uspto-grants-1999_04 |
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| ORD ID | ord-f2c79ed541144f2f96a11b9c267a6001 |
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| 출처 메모 | uspto-grants-1999_04 |
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