反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1Cl)[C:5]([OH:7])=[O:6].[NH2:12][C:13]1[CH:14]=[C:15](B(O)O)[CH:16]=[CH:17][CH:18]=1.C([O-])([O-])=O.[K+].[K+]>CC([O-])=O.CC([O-])=O.[Pd+2].C1(P(C2CCCCC2)C2C=CC=CC=2C2C(OC)=CC=C(S([O-])(=O)=O)C=2OC)CCCCC1.[Na+].O>[NH2:1][C:2]1[CH:3]=[C:4]([C:5]([OH:7])=[O:6])[CH:8]=[CH:9][C:10]=1[C:17]1[CH:16]=[CH:15][CH:14]=[C:13]([NH2:12])[CH:18]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 3
実験手順
The general procedure described in Example 3 was used with 3-amino-4-chloro-benzoic acid (172 mg, 1.00 mmol), 3-aminophenylboronic acid (190 mg, 1.40 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 (552 mg, 4.00 mmol), water (3.0 mL), 12 h, 100° C. The product was isolated as a light brown oil (254 mg, 99%). 1H NMR (400 MHz, CDCl3/d4-MeOH) δ: 7.35 (m, 2H), 7.10 (t, 1H, J=7.6 Hz), 7.02 (d, 1H, J=8.0 Hz), 6.70-6.60 (m, 3H). 13C NMR (125 MHz, CDCl3/d4-MeOH) δ: 169.4, 146.6, 143.4, 139.4, 132.4, 129.9, 129.7, 129.0, 119.8, 118.9, 115.8, 115.5, 114.8. IR (neat, cm−1): 3419, 1645, 1016. EI-MS for C13H12N2O2: Theoretical [M+H]=229.0977. Found: 229.0982. Anal. Calcd for C13H12N2O2: C, 68.41; H, 5.30. Found: C, 68.29; H, 5.29.
出典と根拠
- ORDレコード
- ord-b42a9f4ccafb42b9abd4574aaad385fd
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07560596B2
関連ノート
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