참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 6-Chloroimidazo[1,2-b]pyridazine-2-carboxylic acid | HCID 2794637 | — |
| 반응물 | Ethyl 2-amino-2-methylpropanoate hydrochloride | HCID 22343822 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | N-(6-chloroimidazo[1,2-b]pyridazine-2-carbonyl)-2,2-dimethylglycine ethyl ester | HCID 22989357 | 59.6% |
반응 단계
1.28 g of 6-chloroimidazo[1,2-b]pyridazine-2-carboxylic acid was suspended in 12 ml of N,N-dimethylformamide; 1.16 g of N,N′-carbonyldiimidazole was added, followed by stirring at room temperature for 30 minutes. To the reaction mixture, 1.20 g of 2-aminoisobutyric acid ethyl ester hydrochloride and 1.00 ml of triethylamine were added, followed by stirring at room temperature for 16 hours. Water was added, the crystal precipitated was collected by filtration; the filtrate was extracted with ethyl acetate; the extract was washed with saturated saline, dried over magnesium sulfate and concentrated under reduced pressure. The residue was combined with the above crystal collected by filtration and subjected to silica gel column chromatography and eluted with hexane:ethyl acetate (2:1). The desired fraction was collected and concentrated under reduced pressure to yield 1.20 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-01d2e24ee6a84d2493df929573bd236c |
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| 출처 메모 | uspto-grants-2003_09 |
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