Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 874416생성일: 2026년 10월 25일
Perchloric Acid → 1-amino-4-(methoxycarbonyl)pyridin-2(1H)-iminium 2,4,6-trimethylbenzenesulfonate
https://huagongshe.com/reaction/874416
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Perchloric Acid | HCID 24247 | — |
| 반응물 | Methyl 2-aminopyridine-4-carboxylate | HCID 236984 | — |
| 반응물 | ethyl (1E)-N-{[(2,4,6-trimethylphenyl)sulfonyl]oxy}ethanimidate | HCID 5748625 | — |
| 반응물 | 2-Aminoisonicotinate | HCID 23171621 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | tert-Butyl methyl ether | HCID 15413 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 1-amino-4-(methoxycarbonyl)pyridin-2(1H)-iminium 2,4,6-trimethylbenzenesulfonate | HCID 178498459 | 88.6% |
반응 단계
70% Perchloric acid (18.9 ml) was added to a 1,4-dioxane (26 ml) solution of (Z)-ethyl N-(mesitylsulfonyl)oxyacetimidate (11.7 g) at 4° C. over 20 minutes. Thereafter, the reaction solution was stirred at 3° C. for 30 minutes, and it was then poured into water (100 ml). The precipitated solid was collected by filtration, and was then washed with water (45 ml) to obtain a white solid as a crude product. Methyl 2-aminoisonicotinate (5 g) was added to methylene chloride (35 ml), and the obtained mixture was then cooled to 3° C. The obtained crude product was dissolved in methylene chloride (40 ml), and only an organic layer was added to a methylene chloride solution of 2-aminoisonicotinate. The obtained mixture was stirred at 3° C. for 30 minutes. Thereafter, methyl tert-butyl ether (50 ml) was added to the reaction solution, and the precipitated solid was collected by filtration. The collected solid was washed with methyl tert-butyl ether (20 ml), and was then dried at 45° C., so as to obtain the title compound (10.7 g) in the form of a light yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08980889B2 |
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| 출처 데이터셋 | uspto-grants-2015_03 |
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| ORD ID | ord-f8413180f87045898dcabba00f86e1b7 |
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| 출처 메모 | uspto-grants-2015_03 |
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