참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | O-Benzylhydroxylamine | HCID 102313 | — |
| 반응물 | N-(4,6-dichloro-2-formamido-pyrimidin-5-yl)formamide | HCID 13989892 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 6-Benzyloxyamino-4-chloro-2,5-diformamidopyrimidine | HCID 14523960 | 46.1% |
반응 단계
A mixture of 4,6-dichloro-2,5-diformamido-pyrimidine (1.9 g, 8.09 mmol), benzyloxyamine (1 g, 8.13 mmol), triethylamine (2 ml) and dioxan (20 ml) was stirred at 100° C. for 1 hour. The cooled reaction mixture was filtered and the precipitate collected and washed with dioxan (2×5 ml). The filtrate and washings were combined and evaporated to a syrup. Column chromatography on silica gel (eluted with chloroform-ethanol, 30:1) afforded the title compound (1.2 g, 46%). IR: νmax (KBr) 3242, 1694, 1588, 1472 cm-1 ; 1H NMR δH [(CD3)2SO], 4.89 (2H, s, OCH2Ph), 7.4 (5H, m, Ph), 8.15 (1H, s, CHO), 9.18, 9.42 (1H, 2×br.s, D2O exchangeable, NH), 9.25 (1H, br.s, CHO), 10.91 (2H, br.s, D2O exchangeable, 2×NH). m/e (FAB+ve ion, thioglycerol) MH+ 322.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04910307 |
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| 출처 데이터셋 | uspto-grants-1990_03 |
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| ORD ID | ord-6423771b31554a3bb333f0cf21590763 |
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| 출처 메모 | uspto-grants-1990_03 |
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