参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | 3-氯苯甲酸 | HCID 447 | — |
| 反应物 | 碳酸钾 | HCID 11430 | — |
| 反应物 | 2-氨基苯硼酸 | HCID 2773216 | — |
| 催化剂 | palladium acetate | HCID 167845 | — |
| 催化剂 | 2'-二环己基-2,6-二甲氧基-3-磺酸- 1,1'-联苯水合物钠盐 | HCID 23677046 | — |
| 溶剂 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 产物 | 2-AMINOBIPHENYL-3-CARBOXYLIC ACID | HCID 2772297 | 95.2% |
反应步骤
The general procedure described in Example 3 was used with 3-chlorobenzoic acid (157 mg, 1.00 mmol), 2-aminophenylboronic acid (205 mg, 1.50 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), 12 h, 100° C. The product was isolated as a white solid (203 mg, 95%). Mp=170° C. (lit.=173-175° C.) 1H NMR (400 MHz, d4-MeOH) δ: 8.07 (m, 1H), 7.99 (d, 1H, J=7.6 Hz), 7.65 (d, 1H, J=8.0 Hz), 7.53 (t, 1H, J=7.6 Hz), 7.13 (td, 1H, J=1.6 Hz, J=7.6 Hz), 6.84 (d, 1H, J=8.0 Hz), 6.77 (t, 1H, J=7.6 Hz). 13C NMR (125 MHz, d4-MeOH) δ: 169.9, 145.1, 141.7, 134.8, 132.6, 131.4, 131.4, 130.1, 129.9, 129.5, 128.3, 120.0, 117.6.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 专利号 | US07560596B2 |
|---|
| 来源数据集 | uspto-grants-2009_07 |
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| ORD ID | ord-d7827739e0f94b60bffde464c6065368 |
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| 来源说明 | uspto-grants-2009_07 |
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