関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-Bromo-5-fluoropyridin-2-amine | HCID 16126434 | — |
| 反応物 | B-[6-(cyclohexyloxy)-3-pyridinyl]Boronic acid | HCID 66747855 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 6'-(Cyclohexyloxy)-5-fluoro-3,3'-bipyridin-2-amine | HCID 66748841 | 93.1% |
反応手順
Tetrakis(triphenylphosphine)palladium(0) (36.3 mg) was added to a suspension of 3-bromo-5-fluoropyridin-2-amine (200 mg), 6-(cyclohexyloxy)pyridin-3-ylboronic acid (255 mg) and sodium carbonate (222 mg) in DME (5 mL) and water (1 mL) and the mixture was stirred at 90° C. under nitrogen for 3 hr. Water and EtOAc were added and the organic layer was separated, washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo. The residue was purified by column chromatography (silica gel, eluted with EtOAc in hexane) and washed with IPE to give the title compound (280 mg) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08916551B2 |
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| 出典データセット | uspto-grants-2014_12 |
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| ORD ID | ord-e3fc5272606a4ade93e7d1678a58fd9f |
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| 出典メモ | uspto-grants-2014_12 |
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