Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1169161생성일: 2026년 10월 26일
Fumaric Acid → Ethyl 2-[6-[3-[4-(diphenylmethoxy)piperidino] propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate difumarate
https://huagongshe.com/reaction/1169161
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Fumaric Acid | HCID 444972 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 4-(Diphenylmethoxy)-1-piperidinepropaneamine | HCID 10969393 | — |
| 반응물 | Ethyl 2-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropanoate | HCID 11043751 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Ethyl 2-[6-[3-[4-(diphenylmethoxy)piperidino] propylamino]imidazo[1,2-b]pyridazin-2-yl]-2-methylpropionate difumarate | HCID 69842492 | 78.2% |
반응 단계
4.2 g of 4-(diphenylmethoxy)-1-piperidinepropaneamine and 1.76 g of ethyl 2-(6-chloroimidazo[1,2-b]pyridazin-2-yl)-2-methylpropionate were stirred at 192-200° C. for 3.5 hours. After cooling, an aqueous sodium bicarbonate solution was added thereto and extracted with ethyl acetate. The extract was washed with a brine solution, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to be eluted with ethyl acetate:methanol:triethyl amine (100:5:1). The desired fraction was collected and dissolved in 16 mL of ethyl acetate, and a solution prepared by dissolving 867 mg of fumaric acid in 16 mL of methanol was added thereto, followed by concentration. To the residue was added acetone and the crystals formed were collected by filtration, washed with acetone and dried to provide 2.30 g of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06627630B1 |
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| 출처 데이터셋 | uspto-grants-2003_09 |
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| ORD ID | ord-5e9ee67e05ff44568d4c2222abdaa2da |
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| 출처 메모 | uspto-grants-2003_09 |
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