関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Chlorobenzoic Acid | HCID 447 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Acetylphenylboronic acid | HCID 2734309 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 触媒 | Sodium 2'-(dicyclohexylphosphino)-2,6-dimethoxybiphenyl-3-sulfonate | HCID 23677046 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(2-Acetylphenyl)benzoic acid | HCID 20099953 | 97% |
反応手順
The general procedure described in Example 3 was used with 3-chlorobenzoic acid (157 mg, 1.00 mmol), 2-acetylphenylboronic acid (179 mg, 1.20 mmol), Pd(OAc)2 (2.2 mg, 0.010 mmol, 1 mol %), sodium 2-dicyclohexylphosphino-2′,6′-dimethoxybiphenyl-3′-sulfonate (10.0 mg, 0.020 mmol, 2 mol %), K2CO3 (414 mg, 3.00 mmol), water (2.0 mL), 10 h, 100° C. The product was isolated as a light yellow solid (233 mg, 97%). Mp=143° C. 1H NMR (400 MHz, CDCl3) δ: 12.60 (br-s, 1H), 8.05 (m, 1H), 7.65 (d, 1H, J=7.2 Hz), 7.58-7.55 (m, 3H), 7.49 (d, 1H, J=7.2 Hz), 7.42 (d, 1H, J=7.6 Hz), 2.16 (s, 3H). 13C NMR (125 MHz, CDCl3) δ: 204.3, 172.2, 141.7, 140.7, 139.9, 134.7, 131.5, 131.0, 130.7, 130.3, 129.9, 129.2, 128.7, 128.4, 30.8. IR (neat, cm−1): 3419, 2517, 1686, 1018. Anal. Calcd for C15H12O3: C, 74.99; H, 5.03. Found: C, 75.04; H, 5.06.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560596B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-9403b5aeac1544e7a8b9ad4367fc7838 |
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| 出典メモ | uspto-grants-2009_07 |
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