39859-36-4 2-苯甲酰-4-溴苯胺
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分子式C13H10BrNO2.04水溶解性0.0113 mg/ml ; 0.0000409 mol/l 沸点424.6±35.0 °C (760 mmHg) 溶解度DMF:30mg/mL;DMSO:30mg/mL;乙醇:30mg/mL 酸度系数(pKa)-0.01±0.10 (Predicted) 物理性质: Mp 112-113℃;1H NMR(400MHz, CDCl3): δ5.90-6.25(br s, 2H, D2O可交换), 6.72(d, J=8.80Hz, 1H), 7.37(dd, J=11.7,2.3Hz, 1H), 7.47(t, J=7.8Hz, 2H), 7.51-7.58(m, 2H), 7.59-7.64(m, 2H)参考文献: [1] Journal of Chemical Research - Part S, 2002, #12, p.601-603;[2] Patent: WO2009/91324, 2009, A1;[3] Indian Journal of Chemistry, Section B: Organic Chemistry Including Medicinal Chemistry, 1994, vol.33, #7, p.690-691;[4] Monatshefte fur Chemie, 2009, vol.140, #10, p.1183-1187;[5] Tetrahedron Letters, 2002, vol.43, #39, p.7001-7003;[6] Heteroatom Chemistry, 2005, vol.16, #7, p.637-643;[7] Molecules, 2002, vol.7, #8, p.618-627;[8] Synthetic Communications, 1984, vol.14, #11, p.1053-1058合成路线 3(3. 合成:39859-36-4)
- 步骤: 在N2气氛下,向Schlenk管中加入2-氨基苄腈、芳基亚磺酸钠、Pd(OAc)2、bpy、p-硝基苯磺酸钠,加入THF和H2O,80℃搅拌48小时,经萃取、干燥、柱色谱纯化得到产物。
- 条件: 80℃,THF-H2O混合溶剂,N2气氛,Schlenk技术,反应48小时;
- 收率: 90%;
- 参考文献: [1] Molecules, 2014, vol.19, #5, p.6439-6449