The new room-temperature molten salt was prepared based on LiTFSI[LiNC(SO 2CF 3) 2] with OZO(C 3H 5NO 2) which were not reported in literature. Its thermal and electrochemical properties were studied by differential s...The new room-temperature molten salt was prepared based on LiTFSI[LiNC(SO 2CF 3) 2] with OZO(C 3H 5NO 2) which were not reported in literature. Its thermal and electrochemical properties were studied by differential scanning calorimetry, ac impedance spectroscopy and cyclic voltammertry respectively. The results indicated that the structure symmetry of the molecule was depressed and the extent of charges delocalization was expanded, because of introducing oxygen atom of differential electronegativity in OZO molecule. DSC analysis showed that the LiTFSI-OZO molten salt has the excellent thermal stability and its eutectic temperature is below about 223.15 K. Meanwhile, the conductivity of LiTFSI-OZO molten salt at a molar ratio of 1∶4.5 is 0.75×10 -3 S/cm at 298.15 K and 3.50×10 -3 S/cm at 333.15 K. CV analysis showed that the electrochemical window of the sample is about 4 V.展开更多
The fused triazole derivatives,which is an important inhibitors of the dipeptidyl peptidase-Ⅳ enzyme(DPP-Ⅳ),can be used for the treatment or prevention of type 2 diabetes.A new fused triazole derivatives of 3-oxo-3-...The fused triazole derivatives,which is an important inhibitors of the dipeptidyl peptidase-Ⅳ enzyme(DPP-Ⅳ),can be used for the treatment or prevention of type 2 diabetes.A new fused triazole derivatives of 3-oxo-3-[3-trifluoromethyl-5,6-dihydro[1,2,4]-triazolo[4,3-a]pyrazin-7(8H)-yl]-1-phenylpropan-1-amine was synthesized from 2-chloropyrazine and benzaldehyde by hydrazinolysis,trifluoroacetylation,cyclization,hydrogenation,condensation and deprotection reaction.The structures of the compound and its intermediates were determined by IR,NMR,and MS.展开更多
(±)-1-Methyl-7-oxabicyclo[2.2.1]heptan-2-one (1) is a versatile chiral building block for terpenoids. It could be applied in total synthesis of eudesmanes, agarofurans and norcarotenoids. Compound (±)-1 was ...(±)-1-Methyl-7-oxabicyclo[2.2.1]heptan-2-one (1) is a versatile chiral building block for terpenoids. It could be applied in total synthesis of eudesmanes, agarofurans and norcarotenoids. Compound (±)-1 was reduced to alcohol (±)-2. Compound (±)-2 was esterified with commercial available optically pure (S)-(+)-mandelic acid. The diastereomeric ester mixture was separated with preparative HPLC method. After oxidation of the saponified products of diastereomeric ester (+)-4 and (+)-5 respectively, both optically pure enantiomers of compound 1 were prepared for the first time in four steps with an overall yield of 70%. The absolute configurations of (+)-1 and (-)-1 were determined as (+)-(1R,4S)-1-methyl-7-oxabicyclo[2.2.1] heptan-2-one and (-)-(1S,4R)-1-methyl-7-oxabicyclo[2.2.1] heptan-2-one.展开更多
The complex dimethylgallium- [4-nitro-2- (N-benzo- 15-crown-5 ) - 1 -phenoxide ] (C23H31 N2O7Ga) has been synthesized by the method reported. The crystal X-ray diffraction analysis shows that the crystal belongs to th...The complex dimethylgallium- [4-nitro-2- (N-benzo- 15-crown-5 ) - 1 -phenoxide ] (C23H31 N2O7Ga) has been synthesized by the method reported. The crystal X-ray diffraction analysis shows that the crystal belongs to the triclinic with space group P1, M = 517. 23 and the unit cell parameters: a = 1. 4501 (2), b = 1. 5090(2), c = 1. 3865 (6)nm, a = 105. 58(1 ), β = 117. 26(2), γ = 66. 812(8)°, V= 2. 464546nm3, Z =4, Dc = 1. 39g· cm-3, u = 11. 6cm-1, F(000) = 1080, R = 0. 051, Rw = 0. 064. The coordination number of Ga is four and the gallium atom is located in a distorted tetrahedron structure.展开更多
In this paper,(E)1-phenylpropane-1,2-dione2-[O-(2-oxo-2-phenylacetyl)oxime] was synthesized and its photoinitiation property as a photoinitiator is slso studied.It had the similar performance to other commercial photo...In this paper,(E)1-phenylpropane-1,2-dione2-[O-(2-oxo-2-phenylacetyl)oxime] was synthesized and its photoinitiation property as a photoinitiator is slso studied.It had the similar performance to other commercial photoinitiators when it was cured with UV lamp.But it had the best performance when it was cured with sunlight in the presence of oxygen.展开更多
利用超高效液相色谱-三重四极杆质谱建立了沉积物中6种溴代阻燃剂的分析方法,同时进行了采样分析。以正己烷-二氯甲烷(体积比1∶9)为萃取剂,在100℃下用加速溶剂萃取仪提取沉积物样品,循环3次。萃取液浓缩至2.0 m L,转移至净化柱,用150 ...利用超高效液相色谱-三重四极杆质谱建立了沉积物中6种溴代阻燃剂的分析方法,同时进行了采样分析。以正己烷-二氯甲烷(体积比1∶9)为萃取剂,在100℃下用加速溶剂萃取仪提取沉积物样品,循环3次。萃取液浓缩至2.0 m L,转移至净化柱,用150 m L正己烷-二氯甲烷(体积比1∶2)淋洗。将淋洗液浓缩至近干,加入内标物,定容至1 m L后,用液相色谱-三重四极杆准确定量。方法干重检出限为0.01~0.1 ng/g;替代标回收率为75.6%~98.9%,相对标准偏差为12.0%~13.0%;目标物回收率为70.5%~99.2%,相对标准偏差为2.1%~17.0%。研究区域水体沉积物中的三(2,3-二溴丙基)异氰脲酸酯浓度为未检出~0.14 ng/g,(2,4,6-三溴苯氧基)-1,3,5-三嗪浓度为未检出~0.14 ng/g,十溴二苯醚浓度为0.81~4.36 ng/g,六溴苯浓度为未检出~0.08 ng/g,表明沉积物中新型溴代阻燃剂浓度处于较低水平。展开更多
文摘The new room-temperature molten salt was prepared based on LiTFSI[LiNC(SO 2CF 3) 2] with OZO(C 3H 5NO 2) which were not reported in literature. Its thermal and electrochemical properties were studied by differential scanning calorimetry, ac impedance spectroscopy and cyclic voltammertry respectively. The results indicated that the structure symmetry of the molecule was depressed and the extent of charges delocalization was expanded, because of introducing oxygen atom of differential electronegativity in OZO molecule. DSC analysis showed that the LiTFSI-OZO molten salt has the excellent thermal stability and its eutectic temperature is below about 223.15 K. Meanwhile, the conductivity of LiTFSI-OZO molten salt at a molar ratio of 1∶4.5 is 0.75×10 -3 S/cm at 298.15 K and 3.50×10 -3 S/cm at 333.15 K. CV analysis showed that the electrochemical window of the sample is about 4 V.
文摘The fused triazole derivatives,which is an important inhibitors of the dipeptidyl peptidase-Ⅳ enzyme(DPP-Ⅳ),can be used for the treatment or prevention of type 2 diabetes.A new fused triazole derivatives of 3-oxo-3-[3-trifluoromethyl-5,6-dihydro[1,2,4]-triazolo[4,3-a]pyrazin-7(8H)-yl]-1-phenylpropan-1-amine was synthesized from 2-chloropyrazine and benzaldehyde by hydrazinolysis,trifluoroacetylation,cyclization,hydrogenation,condensation and deprotection reaction.The structures of the compound and its intermediates were determined by IR,NMR,and MS.
文摘(±)-1-Methyl-7-oxabicyclo[2.2.1]heptan-2-one (1) is a versatile chiral building block for terpenoids. It could be applied in total synthesis of eudesmanes, agarofurans and norcarotenoids. Compound (±)-1 was reduced to alcohol (±)-2. Compound (±)-2 was esterified with commercial available optically pure (S)-(+)-mandelic acid. The diastereomeric ester mixture was separated with preparative HPLC method. After oxidation of the saponified products of diastereomeric ester (+)-4 and (+)-5 respectively, both optically pure enantiomers of compound 1 were prepared for the first time in four steps with an overall yield of 70%. The absolute configurations of (+)-1 and (-)-1 were determined as (+)-(1R,4S)-1-methyl-7-oxabicyclo[2.2.1] heptan-2-one and (-)-(1S,4R)-1-methyl-7-oxabicyclo[2.2.1] heptan-2-one.
文摘The complex dimethylgallium- [4-nitro-2- (N-benzo- 15-crown-5 ) - 1 -phenoxide ] (C23H31 N2O7Ga) has been synthesized by the method reported. The crystal X-ray diffraction analysis shows that the crystal belongs to the triclinic with space group P1, M = 517. 23 and the unit cell parameters: a = 1. 4501 (2), b = 1. 5090(2), c = 1. 3865 (6)nm, a = 105. 58(1 ), β = 117. 26(2), γ = 66. 812(8)°, V= 2. 464546nm3, Z =4, Dc = 1. 39g· cm-3, u = 11. 6cm-1, F(000) = 1080, R = 0. 051, Rw = 0. 064. The coordination number of Ga is four and the gallium atom is located in a distorted tetrahedron structure.
文摘In this paper,(E)1-phenylpropane-1,2-dione2-[O-(2-oxo-2-phenylacetyl)oxime] was synthesized and its photoinitiation property as a photoinitiator is slso studied.It had the similar performance to other commercial photoinitiators when it was cured with UV lamp.But it had the best performance when it was cured with sunlight in the presence of oxygen.
文摘利用超高效液相色谱-三重四极杆质谱建立了沉积物中6种溴代阻燃剂的分析方法,同时进行了采样分析。以正己烷-二氯甲烷(体积比1∶9)为萃取剂,在100℃下用加速溶剂萃取仪提取沉积物样品,循环3次。萃取液浓缩至2.0 m L,转移至净化柱,用150 m L正己烷-二氯甲烷(体积比1∶2)淋洗。将淋洗液浓缩至近干,加入内标物,定容至1 m L后,用液相色谱-三重四极杆准确定量。方法干重检出限为0.01~0.1 ng/g;替代标回收率为75.6%~98.9%,相对标准偏差为12.0%~13.0%;目标物回收率为70.5%~99.2%,相对标准偏差为2.1%~17.0%。研究区域水体沉积物中的三(2,3-二溴丙基)异氰脲酸酯浓度为未检出~0.14 ng/g,(2,4,6-三溴苯氧基)-1,3,5-三嗪浓度为未检出~0.14 ng/g,十溴二苯醚浓度为0.81~4.36 ng/g,六溴苯浓度为未检出~0.08 ng/g,表明沉积物中新型溴代阻燃剂浓度处于较低水平。
