関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Bromopropanedial | HCID 74945 | — |
| 反応物 | HCID 178508559 | HCID 178508559 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | {6-Bromo-[1,2,4]triazolo[1,5-a]pyrimidin-2-yl}methanol | HCID 57527274 | — |
反応手順
To a slurry of (5-amino-1H-[1,2,4]triazol-3-yl)-methanol (6.29 g, 33.12 mmol) in acetic acid (25 ml) was added bromomalonaldehyde (5 g, 33.12 mmol). The mixture was heated at 60° C. for hours, and then cooled to room temperature. The light yellow solid was formed. After the solid were removed by filtration followed by drying in vacuum oven provides the light yellow solid as desired product, the filtrate was concentrate by rotary evaporation to give yellow oil. The crude oil was purified by flash chromatography (2% MeOH in CH2Cl2) to give the desired product as light yellow solid (combine total 6.5 g, 86% yield). 1H NMR (300 MHz, DMSO-D6) δ ppm 4.65 (d, J=5.46 Hz, 2 H) 5.50–5.67 (m, 1 H) 8.94 (d, J=2.45 Hz, 1 H) 9.83 (d, J=2.26 Hz, 1 H). MS: (APCI) 230 (M+H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07148226B2 |
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| 出典データセット | uspto-grants-2006_12 |
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| ORD ID | ord-8f33025885764352ad55b8c67a347e91 |
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| 出典メモ | uspto-grants-2006_12 |
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