関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl 2-aminobenzoate | HCID 6877 | — |
| 反応物 | Binap, (A+-)- | HCID 634876 | — |
| 反応物 | Sodium t-butoxide | HCID 23676156 | — |
| 反応物 | 5-Bromo-2-(3-methoxyphenyl)pyridine | HCID 49758519 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ethyl acetate hexane | HCID 21226206 | 98.4% |
| 生成物 | 2-(6-(3-Methoxyphenyl)pyridin-3-ylamino)benzoic acid | HCID 25186999 | — |
反応手順
In a schlenck tube, a mixture of 5-bromo-2-(3-methoxyphenyl)pyridine (Intermediate 27, 0.91 mmol, 0.23 g), ethyl 2-aminobenzoate (Intermediate 33, 0.91 mmol, 0.15 g), BINAP (0.05 mmol, 0.028 g), Pd2(dba)3 (0.05 mmol, 0.042 g) and NaOtBu (1.82 mmol, 0.175 g) in toluene (4 ml) was heated at 110° C. for 12 hours, under argon atmosphere. The solvent was evaporated and the solid residue was triturated with aqueous solution of 2N HCl and extracted with CHCl3. The crude mixture was purified by flash chromatography over SiO2 eluting with mixtures of hexane/ethyl acetate affording 0.078 g (yield 26%) of the expected compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 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-0c6010783c884be28f919b4217d37301 |
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| 出典メモ | uspto-grants-2013_09 |
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