참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1-Benzyl-4-(4-nitrophenyl)piperazine | HCID 2747427 | — |
| 반응물 | Calcium Chloride | HCID 5284359 | — |
| 촉매 | Zinc | HCID 23994 | — |
| 용매 | Acetic acid ethanol water | HCID 86584229 | — |
| 생성물 | 4-(4-Benzylpiperazin-1-yl)aniline | HCID 737259 | 96.7% |
반응 단계
4-(4-Benzyl-1-piperazinyl)-1-nitrobenzene (2.6 g; 8.9 mmol) synthesized by the above process and zinc powder (3.2 g; 48 mmol) were added to a solution of calcium chloride (665 mg; 6.0 mmol) in water-ethanol-acetic acid (12 ml-55 ml-1.2 ml), and the mixture was stirred under reflux for 15 minutes in a bath controlled at 110° C. Insoluble substances were removed from the reaction mixture by suction filtration through Celite, and the filtrate was concentrated under reduced pressure. A saturated aqueous solution of sodium hydrogencarbonate was added to the resultant concentrated residue to conduct extraction with chloroform. The organic layer was dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The thus-obtained crude crystals were recrystallized from benzene-n-hexane to obtain 2.3 g (yield: 96%) of 4-(4-benzyl-1-piperazinyl)aniline as pale brown needles (melting point: 137-138° C.).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06645957B2 |
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| 출처 데이터셋 | uspto-grants-2003_11 |
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| ORD ID | ord-eb341ba792304dabbe20cdd9ec0a2ed7 |
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| 출처 메모 | uspto-grants-2003_11 |
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