참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ethanol | HCID 702 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 반응물 | Ethyl{[(5-{3-[(tert-butoxycarbonyl)amino]phenoxy}pyridin-2-yl)amino]carbonothioyl}carbamate | HCID 91208855 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Tert-butyl {3-[(2-amino[1,2,4]triazolo[1,5-a]pyridin-6-yl)oxy]phenyl}carbamate | HCID 57749279 | 83.9% |
반응 단계
To a solution of hydroxylamine hydrochloride (4.34 g, 62.4 mmol) and N-ethyl-N-isopropylpropan-2-amine (12.7 mL, 72.8 mmol) in methanol (70 mL)/ethanol (70 mL) was added ethyl{[(5-{3-[(tert-butoxycarbonyl)amino]phenoxy}pyridin-2-yl)amino]carbonothioyl}carbamate (4.50 g, 10.4 mmol), and the mixture was stirred with heating at 60° C. for 12 hr. The reaction mixture was concentrated under reduced pressure, and the residue was diluted with ethyl acetate (500 mL), and washed with water (200 mL) and saturated brine (200 mL). The organic layer was dried over anhydrous sodium sulfate, the insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was recrystallized from ethyl acetate, hexane and diisopropyl ether to give the title compound (2.98 g, 83%) as a colorless powder.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08344135B2 |
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| 출처 데이터셋 | uspto-grants-2013_01 |
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| ORD ID | ord-b425bb6533ff4b07a8aabeaa9c9614b1 |
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| 출처 메모 | uspto-grants-2013_01 |
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