関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trichloroisocyanuric Acid | HCID 6909 | — |
| 反応物 | Tempo | HCID 2724126 | — |
| 反応物 | [5-(Propan-2-yloxy)pyridin-2-yl]methanol | HCID 66598374 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 5-Isopropoxypicolinaldehyde | HCID 79794046 | 85% |
反応手順
[5-(1-Methylethoxy)pyridin-2-yl]methanol (30 mg, 0.198 mmol) was dissolved in acetone (2.0 mL). The resultant mixture was added with 2,2,6,6-tetramethylpiperidine 1-oxyl (3.1 mg, 0.020 mmol) and trichloroisocyanuric acid (50 mg, 0.218 mmol) under ice-cold conditions, and stirred at 0° C. for 5 minutes. The reaction solution was concentrated in vacuo, added with an aqueous solution of sodium hydrogen carbonate, and extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate, and concentrated in vacuo. The obtained residue was purified using silica-gel column chromatography (hexane/ethyl acetate), and 5-(1-methylethoxy)picolinaldehyde (25 mg, yield 85%) was obtained as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08153634B2 |
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| 出典データセット | uspto-grants-2012_04 |
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| ORD ID | ord-d27e2569d0024a778adeb343fc81cafa |
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| 出典メモ | uspto-grants-2012_04 |
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