590, 552, 459, 442〇
[0038] UV-vis (DMF),λ max (nm): 328〇
[0039] 1H NMR (400 MHz, CDCl3) δ (ppm) : 8· 05 (d,/= 7· 6 Hz, 2Η),7· 57-7. 54 (m, 1Η), 7.47-7.44 (m, 2Η), 7.11-6.99 (m, 10Η), 3.49 (d, / = 2. I Hz, 3Η), 3.10 (s, 4Η), 2.17 (s, 3Η), 0.93 (q, /=3·7Ηζ, 1Η)〇
[0040] 13C 匪R (100 MHz, CDCl3) δ (ppm) : 174.79, 160.94, 152.91, 136.16, 132.89, 132.07, 128.71, 124.40, 128.19, 125.46, 109.98, 50.84, 33.66, 12.90〇
[0041] 晶體學(xué)數(shù)據(jù):單斜晶系,空間群 Ρ2 (I)/η,a = 1.2237(2) nm,b = 0.94388(15) nm,c = 2.0654(4) nm,α=γ =90°,β =91. 406(2) °,Z=4, V= 2.3850(7) nm3, Dc= 1.496 Mg ·πι3,πι(ΜοΚα)= LKMmm1jF(OOO) = 1088〇
[0042] 實(shí)施例2 : 2-羰基丙酸苯甲酰腙二芐基錫配合物的制備: 在有氮?dú)獗Wo(hù)的IOOmL三口燒瓶中加入0.372g (LOmmol)二芐基二氯化錫、0. 136g (1.0 mmol)苯甲酰肼、0. 116g (I. 05mmol)丙酮酸鈉及35mL溶劑無水甲醇,在溫度為 45~65°C的條件下反應(yīng)5 h,冷卻,過濾,在20~35°C的條件下控制溶劑揮發(fā)結(jié)晶,得淡綠色透 明晶體,即為2-羰基丙酸苯甲酰腙二芐基錫配合物。產(chǎn)率:82. 7%。熔點(diǎn):120~122°C (dec)。
[0043] 元素分析(C25H26N2O4Sn):計算值:C 55. 90, H 4. 88, N 5. 21 ;實(shí)測值:C 55. 84, H 4. 89, N 5. 15〇
[0044] FT-IR (KBr, v/cm 工):3435,3078,3022,2941,1599,1584,1389, 1335, 590,552,459,442。
[0045] UV-vis (DMF),λ max (nm) : 328〇
[0046] 1H NMR (400 MHz, CDCl3) δ (ppm) : 8· 05 (d,/= 7· 6 Hz, 2H),7· 57-7. 54 (m, 1H), 7.47-7.44 (m, 2H), 7.11-6.99 (m, 10H), 3.49 (d, / = 2. I Hz, 3H), 3.10 (s, 4H), 2.17 (s, 3H), 0.93 (q, /=3·7Ηζ, 1Η)〇
[0047] 13C 匪R (100 MHz, CDCl3) δ (ppm) : 174.79, 160.94, 152.91, 136.16, 132.89, 132.07, 128.71, 124.40, 128.19, 125.46, 109.98, 50.84, 33.66, 12.90〇
[0048] 晶體學(xué)數(shù)據(jù):單斜晶系,空間群 P2 (I)/n,a = 1.2237(2) nm,b = 0.94388(15) nm,c = 2.0654(4) nm,α =γ =90°,β =91. 406(2) °,Z=4, V= 2.3850(7) nm3, Dc= 1.496 Mg ·πι3,πι(ΜοΚα)= LKMmm1jF(OOO) = 1088〇
[0049] 實(shí)施例3 : 2-羰基丙酸苯甲酰腙二芐基錫配合物的制備: 在有氮?dú)獗Wo(hù)的IOOmL三口燒瓶中加入0. 372g (1.0 mmol)二芐基二氯化錫、 0.142g (1.05mmol)苯甲酰肼、0.126g (L15mmol)丙酮酸鈉及30mL溶劑無水甲醇,在 溫度為45~65°C的條件下反應(yīng)15 h,冷卻,過濾,在20~35°C的條件下控制溶劑揮發(fā)結(jié)晶, 得淡綠色透明晶體,即為2-羰基丙酸苯甲酰腙二芐基錫配合物。產(chǎn)率:84.0%。熔點(diǎn): 120~122〇C (dec)〇
[0050] 元素分析(C25H26N2O4Sn):計算值:C 55. 90, H 4· 88, N 5· 21 ;實(shí)測值:C 55. 84, H 4· 89, N 5· 15〇
[0051] FT-IR (KBr, ν/cm: 3435, 3078, 3022, 2941,1599, 1584, 1389,1335, 590, 552, 459, 442〇
[0052] UV-vis (DMF),λ max (nm): 328〇
[0053] 1H NMR (400 MHz, CDCl3) δ (ppm) : 8· 05 (d,/= 7· 6 Hz, 2Η),7· 57-7. 54 (m, 1Η), 7.47-7.44 (m, 2Η), 7.11-6.99 (m, 10Η), 3.49 (d, / = 2. I Hz, 3Η), 3.10 (s, 4Η), 2.17 (s, 3Η), 0.93 (q, /=3·7Ηζ, 1Η)〇
[0054] 13C 匪R (100 MHz, CDCl3) δ (ppm) : 174.79, 160.94, 152.91, 136.16, 132.89, 132.07, 128.71, 124.40, 128.19, 125.46, 109.98, 50.84, 33.66, 12.90〇
[0055] 晶體學(xué)數(shù)據(jù):單斜晶系,空間群 Ρ2 (I)/η,a = 1.2237(2) nm,b = 0.94388(15) nm,c = 2.0654(4) nm,α=γ =90°,β =91. 406(2) °,Z=4, V= 2.3850(7) nm3, Dc= 1.496 Mg ·πι3,πι(ΜοΚα)= LKMmm1jF(OOO) = 1088〇
[0056] 實(shí)施例4 : 2-羰基丙酸苯甲酰腙二芐基錫配合物的制備: 在有氮?dú)獗Wo(hù)的250mL三口燒瓶中加入I. 860g (5. Ommol)二芐基二氯化錫、 0.694g (5. Immol)苯甲酰肼、0.594g (5.4mmol)丙酮酸鈉及IOOmL溶劑無水甲醇,在溫 度為45~65°C的條件下反應(yīng)20 h,冷卻,過濾,在20~35°C的條件下控制溶劑揮發(fā)結(jié)晶, 得淡綠色透明晶體,即為2-羰基丙酸苯甲酰腙二芐基錫配合物。產(chǎn)率:81.9%。熔點(diǎn): 120~122 〇C (dec)〇
[0057] 元素分析(C25H26N2O4Sn):計算值:C 55. 90, H 4· 88, N 5· 21 ;實(shí)測值:C 55. 84, H 4· 89, N 5· 15〇
[0058] FT-IR (KBr, ν/cm: 3435, 3078, 3022, 2941,1599, 1584, 1389,1335, 590, 552, 459, 442〇
[0059] UV-vis (DMF),λ max (nm): 328〇
[0060] 1H NMR (400 MHz, CDCl3) δ (ppm) : 8· 05 (d,/= 7· 6 Hz, 2Η),7· 57-7. 54 (m, 1Η), 7.47-7.44 (m, 2Η), 7.11-6.99 (m, 10Η), 3.49 (d, / = 2. I Hz, 3Η), 3.10 (s, 4Η), 2.17 (s, 3Η), 0.93 (q, /=3·7Ηζ, 1Η)〇
[0061] 13C 匪R (100 MHz, CDCl3) δ (ppm) : 174.79, 160.94, 152.91, 136.16, 132.89, 132.07, 128.71, 124.40, 128.19, 125.46, 109.98, 50.84, 33.66, 12.90〇
[0062] 晶體學(xué)數(shù)據(jù):單斜晶系,空間群 Ρ2 (I)/η,a = 1.2237(2) nm,b = 0.94388(15) nm,c = 2.0654(4) nm,α=γ =90°,β =91. 406(2) °,Z=4, V= 2.3850(7) nm3, Dc= 1.496 Mg ·πι3,πι(ΜοΚα)= LKMmm1jF(OOO) = 1088〇
[0063] 實(shí)施例5 : 2-羰基丙酸苯甲酰腙二芐基錫配合物的制備: 在有氮?dú)獗Wo(hù)的250mL三口燒瓶中加入I. 860g (5. Ommol)二芐基二氯化錫、 0.707g (5.2mmol)苯甲酰肼、0.616g (5.6mmol)丙酮酸鈉及150mL溶劑無水甲醇,在溫 度為45~65°C的條件下反應(yīng)22 h,冷卻,過濾,在20~35°C的條件下控制溶劑揮發(fā)結(jié)晶, 得淡綠色透明晶體,即為2-羰基丙酸苯甲酰腙二芐基錫配合物。產(chǎn)率:80.6%。熔點(diǎn): 120~122〇C (dec)〇
[0064] 元素分析(C25H26N2O4Sn):計算值:C 55. 90, H 4· 88, N 5· 21 ;實(shí)測值:C 55. 84, H 4· 89, N 5· 15〇
[0065] FT-IR (KBr, ν/cm: 3435, 3078, 3022, 2941,1599, 1584, 1389,1335, 590, 552, 459, 442〇
[0066] UV-vis (DMF),λ max (nm): 328〇
[0067] 1H NMR (400 MHz, CDCl3) δ (ppm) : 8· 05 (d,/= 7· 6 Hz, 2Η),7· 57-7. 54 (m, 1Η), 7.47-7.44 (m, 2Η), 7.11-6.99 (m, 10Η), 3.49 (d, / = 2. I Hz, 3Η), 3.10 (s, 4Η), 2.17 (s, 3Η), 0.93 (q