The reaction of 3-（3-pyridyl）acrylic acid （H（3-PYA）） with Co（NO3）2.6H2O or MnCl2.4H2O yielded two new complexes： [Co（3-PYA）2（H2O）4.H2O] 1 and [Mn（3-PYA）2（H2O）4] 2. Complex 1 crystallizes in monoclinic...The reaction of 3-（3-pyridyl）acrylic acid （H（3-PYA）） with Co（NO3）2.6H2O or MnCl2.4H2O yielded two new complexes： [Co（3-PYA）2（H2O）4.H2O] 1 and [Mn（3-PYA）2（H2O）4] 2. Complex 1 crystallizes in monoclinic, space group C2/c with a = 9.9473（12）, b = 13.7227（16）, c = 14.7376（18） A, β = 99.043（2）°, V = 1986.7（4） A^3, Z = 4, Dc= 1.549 g/cm^3,μ = 0.921 mm^-1, F（000） = 964, R = 0.0786 and wR = 0.1443. Six types of hydrogen bonds and π-π packing interactions connect the mononuclear units [Co（Ⅱ）（3-PYA）2（H2O）4·H2O] into a three-dimensional supramolecular architecture. Complex 2 crystallizes in monoclinic, space group P21/n with a = 11.3630（16）, b = 7.0346（10）, c = 12.1365（18） A, β = 112.545（3）°, V = 896.0（2） A^3, Z = 2, D, = 1.997 g/cm^3,μ = 0.785 mm^-1, F（000） = 438, R = 0.0787 and wR = 0.1550. The discrete entity Mn（Ⅱ）（3-PYD）2（H2O）4 is extended into a 3-D supramolecular architecture by four kinds of hydrogen bonds.展开更多
Submicrometer-sized, spherical vaterite particles were synthesized by solid-state reaction at room temperature in the presence of poly(acrylic acid)(PAA). The obtained products were characterized by XRD, IR and SEM. I...Submicrometer-sized, spherical vaterite particles were synthesized by solid-state reaction at room temperature in the presence of poly(acrylic acid)(PAA). The obtained products were characterized by XRD, IR and SEM. It was revealed that with increasing PAA amount, the crystal polymorph of CaCO 3 particles varied gradually from pure calcite through a mixture of calcite and vaterite to pure vaterite, and the particle size decreased generally. It was proposed that in solid-state reaction, PAA induced the formation of vaterite and the phase transformation from vaterite to calcite was prevented completely due to the absence of H 2O, resulting in the formation of pure vaterite particles.展开更多
以丙烯酸为原料,采用高温水合制备3-羟基丙酸。探讨了反应温度,丙烯酸浓度,反应时间对收率的影响;确定最佳收率40.2%时的反应条件为:反应温度210℃,丙烯酸浓度4mol/L,反应时间为2h;探讨了高温水合反应的机理及最佳反应部位;测定了3-羟...以丙烯酸为原料,采用高温水合制备3-羟基丙酸。探讨了反应温度,丙烯酸浓度,反应时间对收率的影响;确定最佳收率40.2%时的反应条件为:反应温度210℃,丙烯酸浓度4mol/L,反应时间为2h;探讨了高温水合反应的机理及最佳反应部位;测定了3-羟基丙酸的IR,1 H NMR,13C NMR,均与文献值一致。展开更多
A new method was described for the synthesis of 3-propenolyl-1,3-oxazolidin-2-one.Acrylic acid,triethylamine,and acryloyl chloride were added to anhydrous THF and stirred at -20 for 2 hours,then anhydrous lithium chlo...A new method was described for the synthesis of 3-propenolyl-1,3-oxazolidin-2-one.Acrylic acid,triethylamine,and acryloyl chloride were added to anhydrous THF and stirred at -20 for 2 hours,then anhydrous lithium chloride and 1,3-oxazolidin-2-one were added and stirred at room temperature for 6 hours.The mixture was separated by column chromatohraphy on silica gel to obtain 3-propenolyl-1,3-oxazolidin-2-one,with yield of 83%.展开更多
基金Financially supported by NNSFC (No. 20031020), NSF of Fujian Province and the Key Project from CAS
文摘The reaction of 3-（3-pyridyl）acrylic acid （H（3-PYA）） with Co（NO3）2.6H2O or MnCl2.4H2O yielded two new complexes： [Co（3-PYA）2（H2O）4.H2O] 1 and [Mn（3-PYA）2（H2O）4] 2. Complex 1 crystallizes in monoclinic, space group C2/c with a = 9.9473（12）, b = 13.7227（16）, c = 14.7376（18） A, β = 99.043（2）°, V = 1986.7（4） A^3, Z = 4, Dc= 1.549 g/cm^3,μ = 0.921 mm^-1, F（000） = 964, R = 0.0786 and wR = 0.1443. Six types of hydrogen bonds and π-π packing interactions connect the mononuclear units [Co（Ⅱ）（3-PYA）2（H2O）4·H2O] into a three-dimensional supramolecular architecture. Complex 2 crystallizes in monoclinic, space group P21/n with a = 11.3630（16）, b = 7.0346（10）, c = 12.1365（18） A, β = 112.545（3）°, V = 896.0（2） A^3, Z = 2, D, = 1.997 g/cm^3,μ = 0.785 mm^-1, F（000） = 438, R = 0.0787 and wR = 0.1550. The discrete entity Mn（Ⅱ）（3-PYD）2（H2O）4 is extended into a 3-D supramolecular architecture by four kinds of hydrogen bonds.
文摘Submicrometer-sized, spherical vaterite particles were synthesized by solid-state reaction at room temperature in the presence of poly(acrylic acid)(PAA). The obtained products were characterized by XRD, IR and SEM. It was revealed that with increasing PAA amount, the crystal polymorph of CaCO 3 particles varied gradually from pure calcite through a mixture of calcite and vaterite to pure vaterite, and the particle size decreased generally. It was proposed that in solid-state reaction, PAA induced the formation of vaterite and the phase transformation from vaterite to calcite was prevented completely due to the absence of H 2O, resulting in the formation of pure vaterite particles.
文摘以噻吩-2-甲醛为原料,与磷酰基乙酸三乙酯在氢化钠存在下反应制备3-(2-噻吩)丙烯酸乙酯,后通过水解制备3-(2-噻吩)丙烯酸,总收率78.5%,纯度98.6%,可制备121 g每批。考察了原料滴加速度、物料摩尔比、溶剂用量、柱层析硅胶用量对化合物2合成的影响,确定了最佳条件为:滴加速度8 m L/min、噻吩-2-甲醛与膦酰基乙酸三乙酯摩尔比为1:1.2,溶剂1.6 L,柱层析用硅胶与粗产物重量比为1:15,该步反应收率92.3%,水解后产物经重结晶获得纯品,收率85%。产物结构通过质谱、核磁鉴定正确。
文摘以丙烯酸为原料,采用高温水合制备3-羟基丙酸。探讨了反应温度,丙烯酸浓度,反应时间对收率的影响;确定最佳收率40.2%时的反应条件为:反应温度210℃,丙烯酸浓度4mol/L,反应时间为2h;探讨了高温水合反应的机理及最佳反应部位;测定了3-羟基丙酸的IR,1 H NMR,13C NMR,均与文献值一致。
文摘A new method was described for the synthesis of 3-propenolyl-1,3-oxazolidin-2-one.Acrylic acid,triethylamine,and acryloyl chloride were added to anhydrous THF and stirred at -20 for 2 hours,then anhydrous lithium chloride and 1,3-oxazolidin-2-one were added and stirred at room temperature for 6 hours.The mixture was separated by column chromatohraphy on silica gel to obtain 3-propenolyl-1,3-oxazolidin-2-one,with yield of 83%.
