関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | O-Benzylhydroxylamine | HCID 102313 | — |
| 反応物 | N-(4,6-dichloro-2-formamido-pyrimidin-5-yl)formamide | HCID 13989892 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 6-Benzyloxyamino-4-chloro-2,5-diformamidopyrimidine | HCID 14523960 | 46.1% |
反応手順
A mixture of 4,6-dichloro-2,5-diformamido-pyrimidine (1.9g, 8.09mmol), benzyloxyamine (1g, 8.13mmol), triethylamine (2ml) and dioxan (20ml) was stirred at 100° C. for 1 hour. The cooled reaction mixture was filtered and the precipitate collected and washed with dioxan (2×5ml). 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 (1.2g, 46%). IR: υmax (KBr) 3242, 1694, 1588, 1472cm-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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05159076 |
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| 出典データセット | uspto-grants-1992_10 |
|---|
| ORD ID | ord-fc74fd0fc85443b0abfa1f9ff4ea5c97 |
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| 出典メモ | uspto-grants-1992_10 |
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