関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Cyclopropyl-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 2758015 | — |
| 反応物 | 2-Bromo-5-nitro-3-phenylpyridine | HCID 86657253 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Toluene methanol | HCID 21867641 | — |
| 生成物 | 2-Methoxy-5-nitro-3-phenylpyridine | HCID 46315021 | 60.3% |
反応手順
A mixture of 2-bromo-5-nitro-3-phenylpyridine (0.72 mmol, 0.2 g), 2-cyclopropyl-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (0.86 mmol, 0.16 ml), Pd(PPh3)4 (0.04 mmol, 0.05 g), K2CO3 (2 mmol, 0.28 g) in a toluene/methanol 4:1 mixture (10 ml) was heated at 100° C. for 30 minutes in a microwave, under argon atmosphere. The solvent was evaporated and the crude mixture was extracted between water and ethyl acetate. The solid residue was purified by chromatography over SiO2 eluting with hexane/ethyl acetate mixtures affording 2-methoxy-5-nitro-3-phenylpyridine (0.1 g, yield 55%) of an unexpected product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536165B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-ebc150936cc34ef7a10e84ebc7820aa0 |
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| 出典メモ | uspto-grants-2013_09 |
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