一种2-羰基-2-苯基乙酸水杨酰腙二苯基锡配合物及其制备方法和应用_2

文档序号:9837294阅读:来源:国知局
(m, 10H), 7.02 (td, Ji = 7.5 Hz, J2= 0.9 Hz, 1H), 6.95 (dt, Ji = 8.4 Hz, J2 = 0.9 Hz, 1H), 3.48 (s, 3H), 1.08 (s, lH)〇
[0039] 13C NMR (125 MHz, CDC13) 5(ppm): 176.04, 162.28, 160.81, 150.53, 136.15, 135.48, 135.21, 132.37, 131.75, 130.88, 130.03, 129.62, 128.33, 128.11, 119.46, 117.87, 114.74, 50.81。
[0040] 119Sn NMR (187 MHz, CDC13) δ(ρρπ〇: -307.15。
[0041] 晶体学数据:三斜晶系,空间群P-l,a = 0.9739(4) nm,b = 1.2469(6) nm,c = 1.9945(9) nm,a = 91.654(6)。,β = 91.016(7)。,γ =91.048(7)°,Z=4,V= 2.4203(19) nm3,Dc= 1.611 Mg · m-3,m(MoKa)= 1.099 mm_1,F(000) = 1184〇
[0042] 实施例2: 2-羰基-2-苯基乙酸水杨酰腙二苯基锡配合物的制备: 在有氮气保护的lOOmL三口烧瓶中加入0.344g (1. Ommol)二苯基二氯化锡、0.152g (1 .Ommol)水杨酰肼、0.158g (1.05mmol)苯甲酰甲酸及35mL溶剂无水甲醇,在温度为45~65 °C的条件下反应5 h,冷却,过滤,在20~35°C的条件下控制溶剂挥发结晶,得黄色透明晶体, 即为2-羰基-2-苯基乙酸水杨酰腙二苯基锡配合物。产率:92.3%。熔点:105~106°C (dec)。
[0043] 元素分析((:28!124犯05311):计算值 :〇 57.27,!14.12 4 4.77;实测值:〇 57.34,!1 4·06,Ν 4.79〇
[0044] FT-IR (KBr, v/cm_1): 3608, 3057, 2991, 1693, 1589, 1483, 1452, 1384, 1325, 1255, 1166, 1095, 694, 590, 459〇
[0045] 4 NMR (500 MHz, CDC13) δ(ρρπ〇: 11.42 (s, 1H), 8.23 (dd, Ji = 8.0 Hz, J2 = 1.6 Hz, 1H), 7.78-7.97 (m, 6H), 7.45-7.57 (m, 10H), 7.02 (td, Ji = 7.5 Hz, J2= 0.9 Hz, 1H), 6.95 (dt, Ji = 8.4 Hz, J2 = 0.9 Hz, 1H), 3.48 (s, 3H), 1.08 (s, lH)〇
[0046] 13C NMR (125 MHz, CDC13) 5(ppm): 176.04, 162.28, 160.81, 150.53, 136.15, 135.48, 135.21, 132.37, 131.75, 130.88, 130.03, 129.62, 128.33, 128.11, 119.46, 117.87, 114.74, 50.81。
[0047] 119Sn NMR (187 MHz, CDC13) δ(ρρπ〇: -307.15。
[0048] 晶体学数据:三斜晶系,空间群P-l,a = 0.9739(4) nm,b = 1.2469(6) nm,c = 1.9945(9) nm,a = 91.654(6)。,β = 91.016(7)。,γ =91.048(7)°,Z=4,V= 2.4203(19) nm3,Dc= 1.611 Mg · m-3,m(MoKa)= 1.099 mm_1,F(000) = 1184〇
[0049] 实施例3: 2-羰基-2-苯基乙酸水杨酰腙二苯基锡配合物的制备: 在有氮气保护的l〇〇mL三口烧瓶中加入0.344g (1. Ommol)二苯基二氯化锡、0.160g (1.05mmol)水杨酰肼、0· 173g (1 · 15mmol)苯甲酰甲酸及30mL溶剂无水甲醇,在温度为45~ 65°C的条件下反应15 h,冷却,过滤,在20~35°C的条件下控制溶剂挥发结晶,得黄色透明晶 体,即为2-羰基-2-苯基乙酸水杨酰腙二苯基锡配合物。产率:88.8%。熔点:105~106 °C (dec) 〇
[0050] 元素分析((:28!124犯05311):计算值 :〇 57.27,!14.12 4 4.77;实测值:〇 57.34,!1 4.06, Ν 4.79〇
[0051] FT-IR (KBr, v/cm_1): 3608, 3057, 2991, 1693, 1589, 1483, 1452, 1384, 1325, 1255, 1166, 1095, 694, 590, 459〇
[0052] 4 NMR (500 MHz, CDC13) δ(ρρπ〇: 11.42 (s, 1H), 8.23 (dd, Ji = 8.0 Hz, J2 = 1.6 Hz, 1H), 7.78-7.97 (m, 6H), 7.45-7.57 (m, 10H), 7.02 (td, Ji = 7.5 Hz, J2= 0.9 Hz, 1H), 6.95 (dt, Ji = 8.4 Hz, J2 = 0.9 Hz, 1H), 3.48 (s, 3H), 1.08 (s, lH)〇
[0053] 13C NMR (125 MHz, CDCb) 5(ppm): 176.04, 162.28, 160.81, 150.53, 136.15, 135.48, 135.21, 132.37, 131.75, 130.88, 130.03, 129.62, 128.33, 128.11, 119.46, 117.87, 114.74, 50.81。
[0054] 119Sn NMR (187 MHz, CDCh) δ(ρρπ〇: -307.15。
[0055] 晶体学数据:三斜晶系,空间群P-l,a = 0.9739(4) nm,b = 1.2469(6) nm,c = 1.9945(9) nm,a = 91.654(6)。,β = 91.016(7)。,γ =91.048(7)°,Z=4,V= 2.4203(19) nm3,Dc= 1.611 Mg · m-3,m(MoKa)= 1.099 mm_1,F(000) = 1184〇
[0056] 实施例4: 2-羰基-2-苯基乙酸水杨酰腙二苯基锡配合物的制备: 在有氮气保护的250mL三口烧瓶中加入1.720g (5 . Ommol)二苯基二氯化锡、0.775g (5. lmmol)水杨酰肼、0.810g (5.4mmol)苯甲酰甲酸及100mL溶剂无水甲醇,在温度为45~65 °C的条件下反应20 h,冷却,过滤,在20~35°C的条件下控制溶剂挥发结晶,得黄色透明晶 体,即为2-羰基-2-苯基乙酸水杨酰腙二苯基锡配合物。产率:87.9%。熔点:105~106 °C (dec) 〇
[0057] 元素分析((:28!124犯05311):计算值 :〇 57.27,!14.12 4 4.77;实测值:〇 57.34,!1 4.06, Ν 4.79〇
[0058] FT-IR (KBr, v/cm_1): 3608, 3057, 2991, 1693, 1589, 1483, 1452, 1384, 1325, 1255, 1166, 1095, 694, 590, 459〇
[0059] 4 NMR (500 MHz, CDCh) δ(ρρπ〇: 11.42 (s, 1H), 8.23 (dd, Ji = 8.0 Hz, J2 = 1.6 Hz, 1H), 7.78-7.97 (m, 6H), 7.45-7.57 (m, 10H), 7.02 (td, Ji = 7.5 Hz, J2= 0.9 Hz, 1H), 6.95 (dt, Ji = 8.4 Hz, J2 = 0.9 Hz, 1H), 3.48 (s, 3H), 1.08 (s, lH)〇
[0060] 13C NMR (125 MHz, CDCb) 5(ppm): 176.04, 162.28, 160.81, 150.53, 136.15, 135.48, 135.21, 132.37, 131.75, 130.88, 130.03, 129.62, 128.33, 128.11, 119.46, 117.87, 114.74, 50.81。
[0061] 119Sn NMR (187 MHz, CDC13) δ(ρρπ〇: -307.15。
[0062] 晶体学数据:三斜晶系,空间群P-l,a = 0.9739(4) nm,b = 1.2469(6) nm,c = 1.9945(9) nm,a = 91.654(6)。,β = 91.016(7)。,γ =91.048(7)°,Z=4,V= 2.4203(19) nm3,Dc= 1.611 Mg · m-3,m(MoKa)= 1.099 mm_1,F(000) = 1184〇
[0063] 实施例5: 2-羰基-2-苯基乙酸水杨酰腙二苯基锡配合物的制备: 在有氮气保护的250mL三口烧瓶中加入1.720g (5 . Ommol)二苯基二氯化锡、0.790g (5.2mmol)水杨酰肼、0.840g (5.6mmol)苯甲酰甲酸及150mL溶剂无水甲醇,在温度为45~65 °C的条件下反应22 h,冷却,过滤,在20~35°C的条件下控制溶剂挥发结晶,得黄色透明晶 体,即为2-羰基-2-苯基乙酸水杨酰腙二苯基锡配合物。产率:86.5%。熔点:105~106 °C (dec) 〇
[0064] 元素分析((:28!124犯05311):计算值 :〇 57.27,!14.12 4 4.77;实测值:〇 57.34,!1 4.06, Ν 4.79〇
[0065] FT-IR (KBr, v/cm_1): 3608, 3057, 2991, 1693, 1589, 1483, 1452, 1384, 1325, 1255, 1166, 1095, 694, 590, 459〇
[0066] 4 NMR (500 MHz, CDC13) δ(ρρπ〇: 11.42 (s, 1H), 8.23 (dd, Ji = 8.0 Hz, J2 = 1.6 Hz, 1H), 7.78-7.97 (m, 6H), 7.45-7.57 (m, 10H), 7.02 (td, Ji = 7.5 Hz, J2= 0.9 Hz, 1H), 6.95 (dt, Ji = 8.4 Hz, J2 = 0.9 Hz, 1H), 3.48 (s, 3H), 1.08 (s, lH)〇
[0067] 13C NMR
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